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Sommaire du brevet 3224451 

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Disponibilité de l'Abrégé et des Revendications

L'apparition de différences dans le texte et l'image des Revendications et de l'Abrégé dépend du moment auquel le document est publié. Les textes des Revendications et de l'Abrégé sont affichés :

  • lorsque la demande peut être examinée par le public;
  • lorsque le brevet est émis (délivrance).
(12) Demande de brevet: (11) CA 3224451
(54) Titre français: NOUVEAU SUBSTRAT DE GENERATION D'AEROSOL COMPRENANT L'ESPECE OREGANUM
(54) Titre anglais: NOVEL AEROSOL-GENERATING SUBSTRATE COMPRISING OREGANUM SPECIES
Statut: Demande conforme
Données bibliographiques
(51) Classification internationale des brevets (CIB):
  • A24B 15/14 (2006.01)
  • A24B 15/16 (2020.01)
  • A24B 15/30 (2006.01)
  • A24D 1/18 (2006.01)
  • A24D 1/20 (2020.01)
(72) Inventeurs :
  • ARNDT, DANIEL (Suisse)
  • CAMPANONI, PRISCA (Suisse)
(73) Titulaires :
  • PHILIP MORRIS PRODUCTS S.A.
(71) Demandeurs :
  • PHILIP MORRIS PRODUCTS S.A. (Suisse)
(74) Agent: SMART & BIGGAR LP
(74) Co-agent:
(45) Délivré:
(86) Date de dépôt PCT: 2022-07-14
(87) Mise à la disponibilité du public: 2023-01-19
Licence disponible: S.O.
Cédé au domaine public: S.O.
(25) Langue des documents déposés: Anglais

Traité de coopération en matière de brevets (PCT): Oui
(86) Numéro de la demande PCT: PCT/EP2022/069746
(87) Numéro de publication internationale PCT: EP2022069746
(85) Entrée nationale: 2023-12-28

(30) Données de priorité de la demande:
Numéro de la demande Pays / territoire Date
21186086.1 (Office Européen des Brevets (OEB)) 2021-07-16

Abrégés

Abrégé français

Un article de génération d'aérosol (1000)(4000a, 4000b)(5000) comprend un substrat de génération d'aérosol (1020), le substrat de génération d'aérosol étant constitué d'une substance d'origan homogénéisée comprenant des particules d'origan, d'un agent de formation d'aérosol et d'un liant. Le substrat de génération d'aérosol contient en outre au moins 50 microgrammes d'acide ursolique par gramme du substrat, sur une base de poids sec; au moins 5 microgrammes d'isothymol par gramme du substrat, sur une base de poids sec; et au moins 1,5 microgrammes de thymohydroquinone par gramme du substrat, sur une base de poids sec.


Abrégé anglais

An aerosol-generating article (1000)(4000a,4000b)(5000) comprises an aerosol- generating substrate (1020), the aerosol-generating substrate formed of a homogenised oregano material comprising oregano particles, an aerosol former and a binder. The aerosol- generating substrate further comprises at least 50 micrograms of ursolic acid per gram of the substrate, on a dry weight basis; at least 5 micrograms of isothymol per gram of the substrate, on a dry weight basis; and at least 1.5 micrograms of thymohydroquinone per gram of the substrate, on a dry weight basis.

Revendications

Note : Les revendications sont présentées dans la langue officielle dans laquelle elles ont été soumises.


-68-
CLAIMS
1. An aerosol-generating article comprising an aerosol-generating
substrate, the aerosol-
generating substrate including a homogenised oregano material, the homogenised
oregano
material comprising oregano particles, an aerosol former and a binder, wherein
the aerosol-
generating substrate comprises:
at least 50 micrograms of ursolic acid per gram of the substrate, on a dry
weight basis;
at least 5 micrograms of isothymol per gram of the substrate, on a dry weight
basis; and
at least 1.5 micrograms of thymohydroquinone per gram of the substrate, on a
dry weight
basis.
2. An aerosol-generating article according to claim 1 wherein the amount of
ursolic acid per
gram of the substrate is at least 8 times the amount of isothymol per gram of
the substrate and
wherein the amount of ursolic acid per gram of the substrate is at least 25
times the amount of
thymohydroquinone per gram of the substrate.
3. An aerosol-generating article according to claim 1 or 2, wherein the
aerosol-generating
substrate further comprises between 1 milligram and 20 milligrams of nicotine
per gram of the
substrate, on a dry weight basis.
4. An aerosol-generating article according to any preceding claim, wherein
the
homogenised oregano material comprises between 5 percent by weight and 30
percent by
weight of aerosol former and between 1 percent by weight and 10 percent by
weight of binder,
on a dry weight basis.
5. An aerosol-generating article according to any preceding claim, wherein
the binder
comprises guar gum.
6. An aerosol-generating article according to any preceding claim, wherein
the
homogenised oregano material comprises at least 0.5 percent by weight of the
oregano
particles, on a dry weight basis_
7. An aerosol-generating article according to any preceding claim, wherein
the
homogenised oregano material further comprises tobacco particles and wherein
the weight ratio
of oregano particles to tobacco particles is no more than 1:4.

PCT/EP2022/069746
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8. An aerosol-generating article according to any preceding claim, wherein
the
homogenised oregano material in the aerosol-generating substrate is in the
form of cast leaf.
9. An aerosol-generating article according to any of claims 1 to 7, wherein
the homogenised
oregano material in the aerosol-generating substrate is in the form of oregano
paper.
10. An aerosol-generating article according to any preceding claim, wherein
upon heating of
the aerosol-generating substrate according to Test Method A, an aerosol is
generated
comprising:
at least 1.5 micrograms of ursolic acid per gram of the substrate, on a dry
weight basis;
at least 0.5 microgram of isothymol per gram of the substrate, on a dry weight
basis; and
at least 0.5 microgram of thymohydroquinone per gram of the substrate, on a
dry weight
basis.
11. An aerosol-generating article according to any preceding claim, wherein
upon heating of
the aerosol-generating substrate according to Test Method A, the aerosol
generated from the
aerosol-generating substrate comprises:
ursolic acid in an amount of at least 0.04 micrograms per puff of aerosol;
isothymol in an amount of at least 0.01 micrograms per puff of aerosol; and
thymohydroquinone in an amount of at least 0.01 micrograms per puff of
aerosol,
wherein a puff of aerosol has a volume of 55 millilitres as generated by a
smoking
machine, wherein the amount of ursolic acid per puff of aerosol is at least 2
times the amount of
isothymol per puff of aerosol and wherein the amount of ursolic acid per puff
of aerosol is at
least 2 times the amount of thymohydroquinone per puff of aerosol.
12. An aerosol-generating substrate comprising a homogenised oregano material
comprising oregano particles, aerosol former and binder, wherein the aerosol-
generating
substrate comprises:
at least 50 micrograms of ursolic acid per gram of the substrate, on a dry
weight basis;
at least 5 micrograms of isothymol per gram of the substrate, on a dry weight
basis; and
at least 1.5 micrograms of thymohydroquinone per gram of the substrate, on a
dry weight
basis.
13. An aerosol-generating system comprising:
an aerosol-generating device comprising a heating element; and
an aerosol-generating article according to any of claims 1 to 12.

-70-
14. An aerosol produced upon heating of an aerosol-generating substrate
according to claim
12, the aerosol comprising:
ursolic acid in an amount of at least 0.04 micrograms per puff of aerosol;
isothymol in an amount of at least 0.01 micrograms per puff of aerosol; and
thymohydroquinone in an amount of at least 0.01 micrograms per puff of
aerosol,
wherein a puff of aerosol has a volume of 55 millilitres as generated by a
smoking
machine, wherein the amount of ursolic acid per puff of aerosol is at least 2
times the amount of
isothymol per puff of aerosol and wherein the amount of ursolic acid per puff
of aerosol is at
least 2 times the amount of thymohydroquinone per puff of aerosol.
15. A method of making an aerosol-generating substrate comprising the steps
of:
forming a slurry comprising oregano particles, water, an aerosol former, a
binder and
optionally tobacco particles;
casting or extruding the slurry in the form of a sheet or strands; and
drying the sheet or strands at between 80 and 160 degrees Celsius.

Description

Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.


WO 2023/285597
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NOVEL AEROSOL-GENERATING SUBSTRATE COMPRISING OREGANUM SPECIES
The present invention relates to aerosol-generating substrates comprising
homogenised
plant material formed from oregano particles and to aerosol-generating
articles incorporating
such an aerosol-generating substrate. The present invention further relates to
an aerosol
derived from an aerosol-generating substrate comprising oregano particles.
Aerosol-generating articles in which an aerosol-generating substrate, such as
a tobacco-
containing substrate, is heated rather than combusted, are known in the art.
Typically in such
articles, an aerosol is generated by the transfer of heat from a heat source
to a physically
separate aerosol-generating substrate or material, which may be located in
contact with, within,
around, or downstream of the heat source. During use of the aerosol-generating
article, volatile
compounds are released from the substrate by heat transfer from the heat
source and are
entrained in air drawn through the article. As the released compounds cool,
they condense to
form an aerosol.
Some aerosol-generating articles comprise a flavorant that is delivered to the
consumer
during use of the article to provide a different sensory experience to the
consumer, for example
to enhance the flavour of aerosol. A flavorant can be used to deliver a
gustatory sensation
(taste), an olfactory sensation (smell), or both a gustatory and an olfactory
sensation to the user
inhaling the aerosol. It is known to provide heated aerosol-generating
articles that include
flavorants.
It is also known to provide flavorants in conventional combustible cigarettes,
which are
smoked by lighting the end of the cigarette opposite the mouthpiece so that
the tobacco rod
combusts, generating inhalable smoke. One or more flavorants are typically
mixed with the
tobacco in the tobacco rod in order to provide additional flavour to the
mainstream smoke as the
tobacco is combusted. Such flavorants can be provided, for example, as
essential oil.
Aerosol from a conventional cigarette, which contains a multitude of
components
interacting with receptors located in the mouth provides a sensation of
"mouthfullness," that is
to say, a relatively high mouthfeel. "Mouthfeel," as used herein refers to the
physical sensations
in the mouth caused by food, drink, or aerosol, and is distinct from taste. It
is a fundamental
sensory attribute which, along with taste and smell, determines the overall
flavour of a food item
or aerosol.
There are difficulties involved in replicating the consumer experience
provided by
conventional combustible cigarettes with aerosol-generating articles in which
the aerosol-
generating substrate is heated rather than combusted. This is partially due to
the lower
temperatures reached during the heating of such aerosol-generating articles,
leading to a
different profile of volatile compounds being released.
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It would be desirable to provide a novel aerosol-generating substrate for a
heated aerosol-
generating article providing an aerosol with improved flavour and
mouthfullness. It would be
particularly desirable if such an aerosol-generating substrate could provide
an aerosol with a
sensorial experience that is comparable to that provided by a conventional
combustible
cigarette. It would also be particularly desirable if such an aerosol-
generating substrate could
provide an aerosol that has reduced levels of undesirable aerosol compounds
compared to
existing aerosol-generating substrates, for example those containing tobacco
only.
It would further be desirable to provide such an aerosol-generating substrate
that can be
readily incorporated into an aerosol-generating article and which can be
manufactured using
existing high-speed methods and apparatus.
The present disclosure relates to an aerosol-generating article comprising an
aerosol-
generating substrate, the aerosol-generating substrate formed of a homogenised
plant material
including oregano particles, referred to herein as "homogenised oregano
material". The
homogenised oregano material may further comprise an aerosol former. The
homogenised
oregano material may further comprise a binder. The aerosol-generating
substrate may further
comprise at least about 50 micrograms of ursolic acid per gram of the
substrate, on a dry weight
basis. The aerosol-generating substrate may further comprise at least about 5
micrograms of
isothymol per gram of the substrate, on a dry weight basis. The aerosol-
generating substrate
may further comprise at least about 1.5 micrograms of thymohydroquinone per
gram of the
substrate, on a dry weight basis.
According to the invention there is provided an aerosol-generating article
comprising an
aerosol-generating substrate, the aerosol-generating substrate formed of a
homogenised
oregano material including oregano particles. According to the invention, the
homogenised
oregano material comprises: oregano particles, an aerosol former and a binder.
The aerosol-
generating substrate further comprises at least about 50 micrograms of ursolic
acid per gram of
the substrate, on a dry weight basis; at least about 5 micrograms of isothymol
per gram of the
substrate, on a dry weight basis; and at least about 1.5 micrograms of
thymohydroquinone per
gram of the substrate, on a dry weight basis.
Preferably, upon heating of the aerosol-generating substrate of the aerosol-
generating
article according to the invention according to Test Method A as described
below, an aerosol is
generated comprising: at least about 1.5 micrograms of ursolic acid per gram
of the substrate,
on a dry weight basis; at least about 0.5 microgram of isothymol per gram of
the substrate, on
a dry weight basis; and at least about 0.5 microgram of thymohydroquinone per
gram of the
substrate, on a dry weight basis.
Preferably, upon heating of the aerosol-generating substrate according to Test
Method
A, the aerosol generated from the aerosol-generating substrate may comprise
ursolic acid in an
amount of at least about 0.04 micrograms per puff of aerosol. Upon heating of
the aerosol-
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WO 2023/285597
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-3-
generating substrate according to Test Method A, the aerosol generated from
the aerosol-
generating substrate may comprise isothymol in an amount of at least about
0.01 micrograms
per puff of aerosol. Upon heating of the aerosol-generating substrate
according to Test Method
A, the aerosol generated from the aerosol-generating substrate may comprise
thymohydroquinone in an amount of at least about 0.01 micrograms per puff of
aerosol. A puff
of aerosol has a volume of 55 millilitres as generated by a smoking machine.
According to the invention there is provided an aerosol-generating article
comprising an
aerosol-generating substrate, the aerosol-generating substrate formed of a
homogenised
oregano material including oregano particles. The aerosol-generating substrate
comprises at
least about 50 micrograms of ursolic acid per gram of the substrate, on a dry
weight basis; at
least about 5 micrograms of isothymol per gram of the substrate, on a dry
weight basis; and at
least about 1.5 micrograms of thymohydroquinone per gram of the substrate, on
a dry weight
basis.
The present disclosure also relates to an aerosol-generating substrate formed
of a
homogenised plant material comprising oregano particles, referred to herein as
"homogenised
oregano material". The homogenised oregano material may further comprise an
aerosol former.
The homogenised plant material may further comprise a binder. The aerosol-
generating
substrate may comprise at least about 50 micrograms of ursolic acid per gram
of the substrate,
on a dry weight basis. The aerosol-generating substrate may comprise at least
about 5
micrograms of isothymol per gram of the substrate, on a dry weight basis. The
aerosol-
generating substrate may comprise at least about 1.5 micrograms of
thymohydroquinone per
gram of the substrate, on a dry weight basis.
According to the invention there is also provided an aerosol-generating
substrate formed
of a homogenised oregano material, wherein the homogenised oregano material
comprises
oregano particles, an aerosol former and a binder. The aerosol-generating
substrate further
comprises at least 50 micrograms of ursolic acid per gram of the substrate, on
a dry weight
basis; at least 5 micrograms of isothymol per gram of the substrate, on a dry
weight basis; and
at least 1.5 micrograms of thymohydroquinone per gram of the substrate, on a
dry weight basis.
The present disclosure additionally relates to an aerosol produced upon
heating of an
aerosol-generating substrate. The aerosol may comprise ursolic acid in an
amount of at least
about 0.04 micrograms per puff of aerosol. The aerosol may comprise isothymol
in an amount
of at least about 0.01 micrograms per puff of aerosol. The aerosol may
comprise
thymohydroquinone in an amount of at least about 0.01 micrograms per puff of
aerosol. A puff
of aerosol has a volume of 55 millilitres as generated by a smoking machine.
According to the present invention there is further provided an aerosol
produced upon
heating of an aerosol-generating substrate, the aerosol comprising: ursolic
acid in an amount of
at least about 0.04 micrograms per puff of aerosol; isothymol in an amount of
at least about 0.01
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-4-
micrograms per puff of aerosol; and thymohydroquinone in an amount of at least
about 0.01
micrograms per puff of aerosol, wherein a puff of aerosol has a volume of 55
millilitres as
generated by a smoking machine.
The present invention further provides a method of making an aerosol-
generating
substrate comprising: forming a slurry comprising oregano particles, water, an
aerosol former,
a binder and optionally tobacco particles; casting or extruding the slurry in
the form of a sheet
or strands; and drying the sheets or strands, preferably at a temperature of
between 80 and 160
degrees Celsius. Where a sheet of aerosol-generating substrate is formed, the
sheet may
optionally be cut into strands or gathered the sheet to form a rod. The sheet
may optionally be
crimped prior to the gathering step.
Any references below to the aerosol-generating substrates and aerosols of the
present
invention should be considered to be applicable to all aspects of the
invention, unless stated
otherwise.
As used herein, the term "aerosol-generating article" refers to an article for
producing an
aerosol, wherein the article comprises an aerosol-generating substrate that is
suitable and
intended to be heated or combusted in order to release volatile compounds that
can form an
aerosol. A conventional cigarette is lit when a user applies a flame to one
end of the cigarette
and draws air through the other end. The localised heat provided by the flame
and the oxygen
in the air drawn through the cigarette causes the end of the cigarette to
ignite, and the resulting
combustion generates an inhalable smoke. By contrast, in "heated aerosol-
generating articles",
an aerosol is generated by heating an aerosol-generating substrate and not by
combusting the
aerosol-generating substrate. Known heated aerosol-generating articles
include, for example,
electrically heated aerosol-generating articles and aerosol-generating
articles in which an
aerosol is generated by the transfer of heat from a combustible fuel element
or heat source to a
physically separate aerosol-generating substrate.
Also known are aerosol-generating articles that are adapted to be used in an
aerosol-
generating system that supplies the aerosol former to the aerosol-generating
articles. In such a
system, the aerosol-generating substrate in the aerosol-generating articles
contain substantially
less aerosol former relative to those aerosol-generating substrate which
carries and provides
substantially all the aerosol former used in forming the aerosol during
operation.
As used herein, the term "aerosol-generating substrate" refers to a substrate
capable of
producing upon heating volatile compounds, which can form an aerosol. The
aerosol generated
from aerosol-generating substrates may be visible to the human eye or
invisible and may include
vapours (for example, fine particles of substances, which are in a gaseous
state, that are
ordinarily liquid or solid at room temperature) as well as gases and liquid
droplets of condensed
vapours.
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As used herein, the term "homogenised plant material" encompasses any plant
material
formed by the agglomeration of particles of plant. For example, sheets or webs
of homogenised
plant material for the aerosol-generating substrates of the present invention
may be formed by
agglomerating particles of plant material obtained by pulverising, grinding or
comminuting
oregano plant material and optionally tobacco material such as tobacco leaf
lamina or tobacco
leaf stems. The homogenised plant material may be produced by casting,
extrusion, paper
making processes or other any other suitable processes known in the art.
As used herein, the term "homogenised oregano material" refers to a
homogenised plant
material comprising oregano particles, optionally in combination with tobacco
particles. The
term "homogenised tobacco material" refers to a homogenised plant material
comprising
tobacco particles but no oregano particles, which is therefore not in
accordance with the
invention.
As used herein, the term "oregano particles" encompasses particles derived
from the
leaves of oregano (Oreganum vulgare). Oreganum vulgare L is a flowering plant
of the
Lamiacea family, which is native to western and southwestern Eurasia and the
Mediterranean
region. Oregano is a culinary herb, the leaves of which are commonly used to
provide a distinct
flavour to foods.
By contrast, oregano essential oil is a distillate extracted from the leaves
of the oregano
plant. The primary flavour compounds in the oregano essential oil include
isothymol (carvacrol)
and thymol.
The present invention provides an aerosol-generating article incorporating an
aerosol-
generating substrate formed of a homogenised plant material including oregano
particles,
referred to herein as a homogenised oregano material. The present invention
also provides an
aerosol derived from such an aerosol-generating substrate. The inventors of
the present
invention have found that through the incorporation of oregano particles into
the aerosol-
generating substrate, it is advantageously possible to produce an aerosol
which provides a novel
sensory experience. Such an aerosol provides unique flavours and may provide
an increased
level of mouthfullness.
In addition, the inventors have found that it is advantageously possible to
produce an
aerosol with an improved oregano aroma and flavour compared to the aerosol
produced through
the addition of oregano additives such as oregano oil. Oregano oil (Chemical
Abstracts Service
Registry Number 8007-11-2) is obtained by steam distillation from the leaves
of the oregano
plant and has a composition of flavorants that are different from oregano
particles, presumably
due to the distillation process which may selectively remove or retain certain
flavorants.
I sothymol (carvacrol) is the main constituent of oregano oil and accounts for
up to 75 percent of
the oregano oil.
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Moreover, in certain aerosol-generating substrates provided herein, oregano
particles may
be incorporated at a sufficient level to provide the desired oregano flavour
whilst maintaining
sufficient tobacco material to provide the desired level of nicotine to the
consumer.
Furthermore, it has been surprisingly found that the inclusion of oregano
particles in an
aerosol-generating substrate provides a significant reduction in certain
undesirable aerosol
compounds compared to an aerosol produced from an aerosol-generating substrate
comprising
100 percent tobacco particles without oregano particles. In particular, as
shown below, it has
been surprisingly found that the inclusion of oregano particles in an aerosol-
generating substrate
provides a significant reduction in certain phenol compounds compared to an
aerosol produced
from an aerosol-generating substrate comprising 100 percent tobacco particles
without oregano
particles. Furthermore, this reduction has been found to be greater than would
be expected on
a proportional basis as a result of the reduction in tobacco particles.
The presence of oregano in homogenised plant material (such as cast leaf) can
be
positively identified by DNA barcoding. Methods for performing DNA barcoding
based on the
nuclear gene ITS2, the rbcL and matK system as well as the plastid intergenic
spacer trnH-
psbA, are well known in the art and can be used (Chen S, Yao H, Han J, Liu C,
Song J, et al.
(2010) Validation of the ITS2 Region as a Novel DNA Barcode for Identifying
Medicinal Plant
Species. PLoSONE 5(1): e8613; Hollingsworth PM, Graham SW, Little DP (2011)
Choosing and
Using a Plant DNA Barcode. PLoS ONE 6(5): e19254).
The inventors have carried out a complex analysis and characterisation of the
aerosols
generated from aerosol-generating substrates of the present invention
incorporating oregano
particles and a mixture of oregano and tobacco particles, and a comparison of
these aerosols
with those produced from existing aerosol-generating substrates formed from
tobacco material
without oregano particles. Based on this, the inventors have been able to
identify a group of
"characteristic compounds" that are compounds present in the aerosols and
which have derived
from the oregano particles. The detection of these characteristic compounds
within an aerosol
within a specific range of weight proportion can therefore be used to identify
aerosols that have
derived from an aerosol-generating substrate including oregano particles.
These characteristic
compounds are notably not present in an aerosol generated from tobacco
material.
Furthermore, the proportion of the characteristic compounds within the aerosol
and the ratio of
the characteristic compounds to each other are clearly indicative of the use
of oregano plant
material and not a oregano oil. Similarly, the presence of these
characteristic compounds in
specific proportions within an aerosol-generating substrate is indicative of
the inclusion of
oregano particles in the substrate.
In particular, the defined levels of the characteristic compounds within the
substrate and
the aerosol are specific to the oregano particles present within the
homogenised oregano
material. The level of each characteristic compound is dependent upon the way
in which the
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oregano particles have been processed during production of the homogenised
oregano material.
The level is also dependent upon the composition of the homogenised oregano
material and in
particular, will be affected by the level of other components within the
homogenised oregano
material. The level of the characteristic compounds within the homogenised
oregano material
will be different to the level of the same compound within the starting
oregano material. It will
also be different to the level of the characteristic compounds within
materials containing oregano
particles but that are not in accordance with the invention as defined herein.
In order to carry out the characterisation of the aerosols, the inventors have
made use of
complementary non-targeted differential screening (NTDS) using liquid
chromatography
coupled to high-resolution accurate-mass mass spectrometry (LC-HRAM-MS) in
parallel with
two-dimensional gas chromatography coupled to time-of-flight mass spectrometry
(GCxGC-
TOFMS).
Non-targeted screening (NTS) is a key methodology for characterising the
chemical
composition of complex matrices by either matching unknown detected compound
features
against spectral databases (suspect screening analysis [SSA]), or if no pre-
knowledge matches,
by elucidating the structure of unknowns using e.g. first order fragmentation
(MS/MS) derived
information matched to in silico predicted fragments from compound databases
(non-targeted
analysis [NTA]). It enables the simultaneous measurement and capability for
semi-quantification
of a large number of small molecules from samples using an unbiased approach.
If the focus is on the comparison of two or more aerosol samples, as described
above,
to evaluate any significant differences in chemical composition between
samples in an
unsupervised way or if group related pre-knowledge is available between sample
groups, non-
targeted differential screening (NTDS) may be performed. A complementary
differential
screening approach using liquid chromatography coupled to high-resolution
accurate-mass
mass spectrometry (LC-HRAM-MS) in parallel with two-dimensional gas
chromatography
coupled to time-of-flight mass spectrometry (GCxGC-TOFMS) has been applied in
order to
ensure comprehensive analytical coverage for identifying the most relevant
differences in
aerosol composition between aerosols derived from articles comprising 100% by
weight
oregano as the particulate plant material and those derived from articles
comprising 100% by
weight tobacco as the particulate plant material.
The aerosol was generated and collected using the apparatus and methodology
set out
in detail below.
LC-HRAM-MS analysis was carried out using a Thermo QExactiveTM high resolution
mass spectrometer in both full scan mode and data dependent mode. In total,
three different
methods were applied in order to cover a wide range of substances with
different ionization
properties and compound classes. Samples were analysed using RP chromatography
with
heated electrospray ionisation (HESI) in both positive and negative modes and
with atmospheric
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pressure chemical ionisation (APCI) in positive mode. The methods are
described in: Arndt, D.
eta!, "In depth characterization of chemical differences between heat-not-burn
tobacco products
and cigarettes using LC-H RAM-MS-based
non-targeted differential screening"
(D01:10.13140/RG.2.2.11752.16643); Wachsmuth, C. et al, "Comprehensive
chemical
characterisation of complex matrices through integration of multiple
analytical modes and
databases for LC-H RAM-MS-based non-targeted
screening" (DOI:
10.13140/RG.2.2.12701.61927); and "Buchholz, C. eta!, "Increasing confidence
for compound
identification by fragmentation database and in silica fragmentation
comparison with LC-HRAM-
MS-based non-targeted screening of complex matrices" (DOI:
10.13140/RG.2.2.17944.49927),
all from the 66th ASMS Conference on Mass Spectrometry and Allied Topics, San
Diego, USA
(2018). The methods are further described in: Arndt, D. eta!, "A complex
matrix characterization
approach, applied to cigarette smoke, that integrates multiple analytical
methods and compound
identification strategies for non-targeted liquid chromatography with high-
resolution mass
spectrometry" (DOI: 10. 1002/rcm.8571).
GCxGC-TOFMS analysis was carried out using an Agilent GC Model 6890A or 7890A
instrument equipped with an Auto Liquid Injector (Model 7683B) and a Thermal
Modulator
coupled to a LECO Pegasus 4DTM mass spectrometer with three different methods
for nonpolar,
polar and highly volatile compounds within the aerosol. The methods are
described in:
Almstetter et al, "Non-targeted screening using GCxGC-TOFMS for in-depth
chemical
characterization of aerosol from a heat-not-burn tobacco product" (DOI:
10.13140/RG.2.2.36010.31688/1); and Almstetter et al, "Non-targeted
differential screening of
complex matrices using GCxGC-TOFMS for comprehensive characterization of the
chemical
composition and determination of significant differences" (DOI:
10.13140/RG.2.2.32692.55680),
from the 66th and 64th ASMS Conferences on Mass Spectrometry and Allied
Topics, San Diego,
USA, respectively.
The results from the analysis methods provided information regarding the major
compounds responsible for the differences in the aerosols generated by such
articles. The focus
of the non-targeted differential screening using both analytical platforms LC-
HRAM-MS and
GCxGC-TOFMS was on compounds that were present in greater amounts in the
aerosols of a
sample of an aerosol-generating substrate according to the invention
comprising 100 percent
oregano particles relative to a comparative sample of an aerosol-generating
substrate
comprising 100 percent tobacco particles. The NTDS methodology is described in
the papers
listed above.
Based on this information, the inventors were able to identify specific
compounds within
the aerosol that may be considered as "characteristic compounds" deriving from
the oregano
particles in the substrate. Characteristic compounds derived from oregano
include but are not
limited to: ursolic acid, (3[3-Hydroxyurs-12-en-28-oic acid), chemical
formula: C30H4803,
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Chemical Abstracts Service Registry Number 77-52-1); isothymol, also known as
carvacrol or
cymophenol, (2-Methyl-5-(propan-2-yl)phenol), chemical formula: C10hl140,
Chemical Abstracts
Service Registry Number 499-75-2); and thymohydroqui none, (2-methy1-5-propan-
2-ylbenzene-
1,4-diol), chemical formula: C10hl1402, Chemical Abstracts Service Registry
Number 2217-60-
9).
For the purposes of the present invention, a targeted screening can be
conducted on a
sample of aerosol-generating substrate to identify the presence and amount of
each of the
characteristic compounds in the substrate. Such a targeted screening method is
described
below. As described, the characteristic compounds can be detected and measured
in both the
aerosol-generating substrate and the aerosol derived from the aerosol-
generating substrate.
As defined above, the aerosol-generating article of the invention comprises an
aerosol-
generating substrate formed of a homogenised plant material comprising oregano
particles. As
a result of the inclusion of the oregano particles, the aerosol-generating
substrate comprises
certain proportions of the "characteristic compounds" of oregano, as described
above. In
particular, the aerosol-generating substrate preferably comprises at least 50
micrograms of
ursolic acid per gram of the substrate, at least 5 micrograms of isothymol per
gram of the
substrate, and at least 1.5 micrograms of thymohydroquinone per gram of the
substrate, on a
dry weight basis.
By defining an aerosol-generating substrate with respect to the desired levels
of the
characteristic compounds, it is possible to ensure consistency between
products despite
potential differences in the levels of the characteristic compounds in the raw
materials. This
advantageously enables the quality of the product to be controlled more
effectively.
Preferably, the aerosol-generating substrate comprises at least about 200
micrograms of
ursolic acid per gram of the substrate, more preferably at least about 500
micrograms of ursolic
acid per gram of the substrate, on a dry weight basis. Alternatively or in
addition, the aerosol-
generating substrate preferably comprises no more than about 6500 micrograms
of ursolic acid
per gram of the substrate, more preferably no more than about 4000 micrograms
of ursolic acid
per gram of the substrate, more preferably no more than about 2500 micrograms
of ursolic acid
per gram of the substrate, on a dry weight basis.
For example, the aerosol-generating substrate may comprise between about 50
micrograms and about 6500 micrograms of ursolic acid per gram of the
substrate, or between
about 200 micrograms and about 4000 micrograms of ursolic acid per gram of the
substrate, or
between about 500 micrograms and about 2500 micrograms of ursolic acid per
gram of the
substrate, on a dry weight basis.
In certain particularly preferred embodiments, the aerosol-generating
substrate may
comprise between about 1000 micrograms and about 2000 micrograms ursolic acid
per gram
of the aerosol-generating substrate, more preferably between about 1200
micrograms and about
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1800 micrograms ursolic acid per gram of the aerosol-generating substrate. For
example, the
level of ursolic acid may be within these ranges for preferred embodiments of
the invention in
which the aerosol-generating substrate comprises between 15 percent by weight
and 20 percent
by weight of oregano particles, on a dry weight basis.
Preferably, the aerosol-generating substrate comprises at least about 50
micrograms of
isothymol per gram of the substrate, more preferably at least about 100
micrograms of isothymol
per gram of the substrate, on a dry weight basis. Alternatively or in
addition, the aerosol-
generating substrate preferably comprises no more than about 600 micrograms of
isothymol per
gram of the substrate, more preferably no more than about 400 micrograms of
isothymol per
gram of the substrate, more preferably no more than about 250 micrograms of
isothymol per
gram of the substrate, on a dry weight basis.
For example, the aerosol-generating substrate may comprise between about 5
micrograms and about 600 micrograms of isothymol per gram of the substrate, or
between about
50 micrograms and about 400 micrograms of isothymol per gram of the substrate,
or between
about 100 micrograms and about 250 micrograms of isothymol per gram of the
substrate, on a
dry weight basis.
In certain particularly preferred embodiments, the aerosol-generating
substrate may
comprise between about 100 micrograms and about 200 micrograms of isothymol
per gram of
the aerosol-generating substrate, more preferably between about 120 micrograms
and about
160 micrograms of isothymol per gram of the aerosol-generating substrate. For
example, the
level of isothymol may be within these ranges for preferred embodiments of the
invention in
which the aerosol-generating substrate comprises between 15 percent by weight
and 20 percent
by weight of oregano particles, on a dry weight basis.
Preferably, the aerosol-generating substrate comprises at least about 10
micrograms of
thymohydroquinone per gram of the substrate, more preferably at least about 25
micrograms of
thymohydroquinone per gram of the substrate, on a dry weight basis.
Alternatively or in addition,
the aerosol-generating substrate preferably comprises no more than about 200
micrograms of
thymohydroquinone per gram of the substrate, more preferably no more than
about 150
micrograms of thymohydroquinone per gram of the substrate, more preferably no
more than
about 100 micrograms of thymohydroquinone per gram of the substrate, on a dry
weight basis.
For example, the aerosol-generating substrate may comprise between about 1.5
micrograms and about 200 micrograms of thymohydroquinone per gram of the
substrate, or
between about 10 microgram and about 150 micrograms of thymohydroquinone per
gram of the
substrate, or between about 25 micrograms and about 100 micrograms of
thymohydroquinone
per gram of the substrate, on a dry weight basis.
In certain particularly preferred embodiments, the aerosol-generating
substrate may
comprise between about 20 micrograms and about 60 micrograms of
thymohydroquinone per
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gram of the aerosol-generating substrate, more preferably between about 30
micrograms and
about 50 micrograms of thymohydroquinone per gram of the aerosol-generating
substrate. For
example, the level of thymohydroquinone may be within these ranges for
preferred
embodiments of the invention in which the aerosol-generating substrate
comprises between 15
percent by weight and 20 percent by weight of oregano particles, on a dry
weight basis.
Preferably, the ratio of the characteristic compounds in the aerosol-
generating substrate
is such that the amount of ursolic acid per gram of the substrate is at least
8 times the amount
of isothymol per gram of the substrate, more preferably at least 10 times the
amount of isothymol
per gram of the substrate.
Preferably, the ratio of the characteristic compounds in the aerosol-
generating substrate
is such that the amount of ursolic acid per gram of the substrate is at least
25 times the amount
of thymohydroquinone per gram of the substrate, more preferably at least 30
times the amount
of thymohydroquinone per gram of the substrate.
These ratios of ursolic acid to isothymol and thymohydroquinone are
characteristic of the
inclusion of oregano particles in the aerosol-generating substrate.
As defined above, the invention also provides an aerosol-generating article
that comprises
an aerosol-generating substrate formed of a homogenised plant material
comprising oregano
particles, wherein upon heating of the aerosol-generating substrate, an
aerosol is generated
which comprises the "characteristic compounds" of oregano.
For the purposes of the invention, the aerosol-generating substrate is heated
according to
"Test Method A". In Test Method A, an aerosol-generating article incorporating
the aerosol-
generating substrate is heated in a Tobacco Heating System 2.2 holder (THS2.2
holder) under
the Health Canada machine-smoking regimen. For the purposes of carrying out
Test Method
A, the aerosol-generating substrate is provided in an aerosol-generating
article that is
compatible with the THS2.2 holder.
The Tobacco Heating System 2.2 holder (THS2.2 holder) corresponds to the
commercially
available IQOS device (Philip Morris Products SA, Switzerland) as described in
Smith et al.,
2016, Regul. Toxicol. Pharmacol. 81 (S2) S82-S92. Aerosol-generating articles
for use in
conjunction with the IQOS device are also commercially available.
The Health Canada smoking regimen is a well-defined and accepted smoking
protocol as
defined in Health Canada 2000 ¨ Tobacco Products Information Regulations
SOR/2000-273,
Schedule 2; published by Ministry of Justice Canada. The test method is
described in ISO/TR
19478-1:2014. In a Health Canada smoking test, an aerosol is collected from
the sample
aerosol-generating substrate over 12 puffs with a puff volume of 55
millimetres, puff duration of
2 seconds and puff interval of 30 seconds, with all ventilation blocked if
ventilation is present.
Thus, in the context of the present invention, the expression "upon heating of
the aerosol-
generating substrate according to Test Method A" means upon heating of the
aerosol-generating
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substrate in a THS2.2 holder under the Health Canada machine-smoking regimen
as defined in
Health Canada 2000 ¨ Tobacco Products Information Regulations SOR/2000-273,
Schedule 2;
published by Ministry of Justice Canada, the test method being described in
ISO/TR 19478-
1:2014.
For the purposes of analysis, the aerosol generated from the heating of the
aerosol-
generating substrate is trapped using suitable apparatus, depending upon the
method of
analysis that is to be used. In a suitable method for generating samples for
analysis by LC-
HRAM-MS, the particulate phase is trapped using a conditioned 44mm Cambridge
glass fiber
filter pad (according to ISO 3308) and a filter holder (according to ISO 4387
and ISO 3308). The
remaining gas phase is collected downstream from the filter pad using two
consecutive micro-
impingers (20mL) containing methanol and internal standard (ISTD) solution
(10mL) each,
maintained at -60 degrees Celsius, using a dry ice-isopropanol mixture. The
trapped particulate
phase and gas phase are then recombined and extracted using the methanol from
the micro-
impingers, by shaking the sample, vortexing for 5 minutes and centrifuging
(4500 g, 5 minutes,
10 degrees Celsius). The resultant extract is diluted with methanol and mixed
in an Eppendorf
ThermoMixer (5 degrees Celsius, 2000 rpm). Test samples from the extract are
analysed by
LC-HRAM-MS in combined full scan mode and data dependent fragmentation mode
for
identification of the characteristic compounds. For the purposes of the
invention, LC-HRAM-MS
analysis is suitable for the identification and quantification of ursolic
acid.
Samples for analysis by GCxGC-TOFMS may be generated in a similar way but for
GCxGC-TOFMS analysis, different solvents are suitable for extracting and
analysing polar
compounds, non-polar compounds and volatile compounds separated from whole
aerosol.
For non-polar and polar compounds, whole aerosol is collected using a
conditioned 44
mm Cambridge glass fiber filter pad (according to ISO 3308) and a filter
holder (according to
ISO 4387 and ISO 3308), followed by two micro-impingers connected and sealed
in series.
Each micro-impinger (20mL) contains 10mL dichloromethane/methanol (80:20 v/v)
containing
internal standard (ISTD) and retention index marker (RIM) compounds. The micro-
impingers
are maintained at -80 degrees Celsius, using a dry ice-isopropanol mixture.
For analysis of the
non-polar compounds, the particulate phase of the whole aerosol is extracted
from the glass
fiber filter pad using the contents of the micro-impingers. Water is added to
an aliquot (10mL)
of the resulting extract and the sample is shaken and centrifuged as described
above. The
dichloromethane layer is separated, dried with sodium sulphate and analysed by
GCxGC-
TOFMS in full scan mode. For analysis of the polar compounds, the remaining
water layer from
the non-polar sample preparation described above is used. ISTD and RIM
compounds are
added to the water layer, which is then directly analysed by GCxGC-TOFMS in
full scan mode.
For volatile compounds, whole aerosol is collected using two micro-impingers
(20mL)
connected and sealed in series, each filled with 10mL N,N-dimethylformamide
(DMF) containing
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ISTD and RIM compounds. The micro-impingers are maintained at between -50 and -
60
degrees Celsius using a dry ice-isopropanol mixture. After collection, the
contents of the two
micro-impingers are combined and analysed by GCxGC-TOFMS in full scan mode.
For the purposes of the invention, GCxGC-TOFMS analysis is suitable for the
identification
and quantification of isothymol and thymohydroquinone.
The aerosol generated upon heating of the aerosol-generating substrate of the
invention
according to Test Method A is preferably characterised by the amounts and
ratios of the
characteristic compounds, ursolic acid, isothymol and thymohydroquinone, as
defined above.
Preferably, in an aerosol-generating article comprising an aerosol-generating
substrate as
described above, upon heating the aerosol-generating substrate according to
Test Method A,
an aerosol is generated comprising at least 1.5 micrograms of ursolic acid per
gram of the
substrate, on a dry weight basis; at least 0.5 microgram of isothymol per gram
of the substrate,
on a dry weight basis; and at least 0.5 micrograms of thymohydroquinone per
gram of the
substrate, on a dry weight basis.
The ranges define the amount of each of the characteristic compounds in the
aerosol
generated per gram of the aerosol-generating substrate (also referred to
herein as the
"substrate"). This equates to the total amount of the characteristic compound
measured in the
aerosol collected during Test Method A, divided by the dry weight of the
aerosol-generating
substrate prior to heating.
Upon heating of the aerosol-generating substrate according to Test Method A,
an aerosol
is preferably generated that preferably comprises at least about 10 micrograms
of ursolic acid
per gram of the substrate, on a dry weight basis. More preferably, the aerosol
generated from
an aerosol-generating substrate according to the present invention comprises
at least about 25
micrograms of ursolic acid per gram of the substrate, on a dry weight basis.
Alternatively, or in addition, the aerosol generated from the aerosol-
generating substrate
preferably comprises up to about 200 micrograms of ursolic acid per gram of
the substrate, on
a dry weight basis. More preferably, the aerosol generated from the aerosol-
generating
substrate comprises up to about 150 micrograms of ursolic acid per gram of the
substrate, on a
dry weight basis. Even more preferably, the aerosol generated from the aerosol-
generating
substrate comprises up to about 100 micrograms of ursolic acid per gram of the
substrate, on a
dry weight basis.
Upon heating of the aerosol-generating substrate according to Test Method A,
an aerosol
is generated that preferably comprises at least about 5 micrograms of
isothymol per gram of the
substrate, on a dry weight basis. More preferably, the aerosol generated from
an aerosol-
generating substrate according to the present invention comprises at least
about 10 micrograms
of isothymol per gram of the substrate, on a dry weight basis.
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Alternatively, or in addition, the aerosol generated from the aerosol-
generating substrate
preferably comprises up to about 50 micrograms of isothymol per gram of the
substrate, on a
dry weight basis. More preferably, the aerosol generated from the aerosol-
generating substrate
comprises up to about 35 micrograms of isothymol per gram of the substrate, on
a dry weight
basis. Even more preferably, the aerosol generated from the aerosol-generating
substrate
comprises up to about 25 micrograms of isothymol per gram of the substrate, on
a dry weight
basis.
Upon heating of the aerosol-generating substrate according to Test Method A,
an aerosol
is generated that preferably comprises at least about 5 microgram of
thymohydroquinone per
gram of the substrate, on a dry weight basis. More preferably, the aerosol
generated from an
aerosol-generating substrate according to the present invention comprises at
least about 10
micrograms of thymohydroquinone per gram of the substrate, on a dry weight
basis.
Alternatively, or in addition, the aerosol generated from the aerosol-
generating substrate
preferably comprises up to about 50 micrograms of thymohydroquinone per gram
of the
substrate, on a dry weight basis. More preferably, the aerosol generated from
the aerosol-
generating substrate comprises up to about 35 micrograms of thymohydroquinone
per gram of
the substrate, on a dry weight basis. Even more preferably, the aerosol
generated from the
aerosol-generating substrate comprises up to about 25 micrograms of
thymohydroquinone per
gram of the substrate, on a dry weight basis.
Preferably, the aerosol produced from an aerosol-generating substrate
according to the
present invention during Test Method A further comprises at least about 0.1
micrograms of
nicotine per gram of the substrate, more preferably at least about 1 microgram
of nicotine per
gram of the substrate, more preferably at least about 2 micrograms of nicotine
per gram of the
substrate, on a dry weight basis. Preferably, the aerosol comprises up to
about 10 micrograms
of nicotine per gram of the substrate, more preferably up to about 7.5
micrograms of nicotine
per gram of the substrate, more preferably up to about 4 micrograms of
nicotine per gram of the
substrate, on a dry weight basis. For example, the aerosol may comprise
between about 0.1
micrograms and about 10 micrograms of nicotine per gram of the substrate, or
between about
1 microgram and about 7.5 micrograms of nicotine per gram of the substrate, or
between about
2 micrograms and about 4 micrograms of nicotine per gram of the substrate, on
a dry weight
basis. In some embodiments of the present invention, the aerosol may contain
zero micrograms
of nicotine.
Various methods known in the art can be applied to measure the amount of
nicotine in
the aerosol.
Alternatively or in addition, the aerosol produced from an aerosol-generating
substrate
according to the present invention during Test Method A may optionally further
comprise at least
about 20 milligrams of a cannabinoid compound per gram of the substrate, more
preferably at
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least about 50 milligrams of a cannabinoid compound per gram of the substrate,
more preferably
at least about 100 milligrams of a cannabinoid compound per gram of the
substrate, on a dry
weight basis. Preferably, the aerosol comprises up to about 250 milligrams of
a cannabinoid
compound per gram of the substrate, more preferably up to about 200 milligrams
of a
cannabinoid compound per gram of the substrate, more preferably up to about
150 milligrams
of a cannabinoid compound per gram of the substrate, on a dry weight basis.
For example, the
aerosol may comprise between about 20 milligrams and about 250 milligrams of a
cannabinoid
compound per gram of the substrate, or between about 50 milligrams and about
200 milligrams
of a cannabinoid compound per gram of the substrate, or between about 100
milligrams and
about 150 milligrams of a cannabinoid compound per gram of the substrate, on a
dry weight
basis. In some embodiments of the present invention, the aerosol may contain
zero micrograms
of cannabinoid compound.
Preferably, the cannabinoid compound is selected from CBD and THC. More
preferably,
the cannabinoid compound is CBD.
Various methods known in the art can be applied to measure the amount of a
cannabinoid compound in the aerosol.
Carbon monoxide may also be present in the aerosol generated from an aerosol-
generating substrate according to the invention during Test Method A and may
be measured
and used to further characterise the aerosol. Oxides of nitrogen such as
nitric oxide and nitrogen
dioxide may also be present in the aerosol and may be measured and used to
further
characterise the aerosol.
According to the present invention, the aerosol generated from the aerosol-
generating
substrate during Test Method A preferably has an amount of ursolic acid per
gram of the
substrate that is at least 2 times the amount of isothymol per gram of the
substrate. The ratio
of ursolic acid to isothymol is therefore at least 2:1. More preferably, the
amount of ursolic acid
in the aerosol generated from the aerosol-generating substrate during Test
Method A is at least
3 times the amount of isothymol per gram of the substrate, such that the ratio
of ursolic acid to
isothymol is at least 3:1.
According to the present invention, the aerosol generated from the aerosol-
generating
substrate during Test Method A preferably has an amount of ursolic acid per
gram of the
substrate that is at least 2 times the amount of thymohydroquinone per gram of
the substrate.
The ratio of ursolic acid to thymohydroquinone is therefore at least 2:1. More
preferably, the
amount of ursolic acid in the aerosol generated from the aerosol-generating
substrate during
Test Method A is at least 3 times the amount of thymohydroquinone per gram of
the substrate,
such that the ratio of ursolic acid to thymohydroquinone is at least 3:1.
The defined ratios of ursolic acid to isothymol and thymohydroquinone
characterise an
aerosol that is derived from oregano particles. In contrast, in an aerosol
produced from oregano
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oil, the ratios of ursolic acid to isothymol and thymohydroquinone would be
significantly
different.
The aerosol produced from an aerosol-generating substrate according to the
invention
during Test Method A may further comprise at least about 5 milligrams of
aerosol former per
gram of aerosol-generating substrate, or at least about 10 milligrams of
aerosol per gram of the
substrate or at least about 15 milligrams of aerosol former per gram of the
substrate.
Alternatively or in addition, the aerosol may comprises up to about 30
milligrams of aerosol
former per gram of the substrate, or up to about 25 milligrams aerosol former
per gram of the
substrate, or up to about 20 milligrams aerosol former per gram of the
substrate. For example,
the aerosol may comprise between about 5 milligrams and about 30 milligrams of
aerosol former
per gram of the substrate, or between about 10 milligrams and about 25
milligrams of aerosol
former per gram of the substrate, or between about 15 milligrams and about 20
milligrams of
aerosol former per gram of the substrate. In alternative embodiments, the
aerosol may comprise
less than 5 milligrams of aerosol former per gram of substrate. This may be
appropriate, for
example, if an aerosol former is provided separately within the aerosol-
generating article or
aerosol-generating device.
Suitable aerosol formers for use in the present invention are set out below.
Various methods known in the art can be applied to measure the amount of
aerosol
former in the aerosol.
As described above, the presence of the characteristic compounds in the
aerosol in the
amounts and ratios defined is indicative of the inclusion of oregano particles
in the homogenised
plant material forming the aerosol-generating substrate.
Preferably, the aerosol-generating substrate according to the invention
comprises
homogenised oregano material comprising at least about 0.5 percent by weight
of oregano
particles, on a dry weight basis. Preferably, the homogenised oregano material
comprises at
least about 0.75 percent by weight of oregano particles, more preferably at
least about 1.5
percent by weight of oregano particles, more preferably at least about 2.5
percent by weight of
oregano particles more preferably at least about 3 percent by weight of
oregano particles, more
preferably at least about 4 percent by weight of oregano particles, more
preferably at least about
5 percent by weight of oregano particles, more preferably at least about 6
percent by weight of
oregano particles, more preferably at least about 7 percent by weight of
oregano particles, more
preferably at least about 8 percent by weight of oregano particles, more
preferably at least about
9 percent by weight of oregano particles, more preferably at least about 10
percent by weight of
oregano particles, on a dry weight basis.
In certain embodiments of the invention, the plant particles forming the
homogenised
oregano material may include at least 99.5 percent by weight of oregano
particles or at least 95
percent by weight of oregano particles or at least 90 percent by weight of
oregano particles,
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based on dry weight of the plant particles. In such embodiments, the aerosol-
generating
substrate therefore comprises oregano particles, with substantially no other
plant particles. For
example, the plant particles forming the homogenised oregano material may
comprise about
100 percent by weight of oregano particles.
In alternative embodiments of the invention, the homogenised oregano material
may
comprise oregano particles in combination with at least one of tobacco
particles or cannabis
particles, as described below.
In the following description of the invention, the term "particulate plant
material" is used to
refer collectively to the particles of plant material that are used to form
the homogenised plant
material. The particulate plant material may consist substantially of oregano
particles or may
be a mixture of oregano particles with tobacco particles, cannabis particles,
or both tobacco
particles and cannabis particles.
The homogenised oregano material may comprise up to about 100 percent by
weight of
oregano particles, on a dry weight basis. Preferably, the homogenised oregano
material
comprises up to about 90 percent by weight of oregano particles, more
preferably up to about
80 percent by weight of oregano particles, more preferably up to about 70
percent by weight of
oregano particles, more preferably up to about 60 percent by weight of oregano
particles, more
preferably up to about 50 percent by weight of oregano particles, on a dry
weight basis.
For example, the homogenised oregano material may comprise between about 0.5
percent and about 100 percent by weight of oregano particles, or about 2.5
percent and about
90 percent by weight of oregano particles, or between about 10 percent and
about 80 percent
by weight of oregano particles, or between about 15 percent and about 70
percent by weight of
oregano particles, or between about 20 percent and about 60 percent by weight
of oregano
particles, or between about 30 percent and about 50 percent by weight of
oregano particles, on
a dry weight basis.
In certain particularly preferred embodiments of the invention, the
homogenised oregano
material comprises between about 15 percent by weight and about 20 percent by
weight of
oregano particles, on a dry weight basis.
As described above, the inventors have identified a number of "characteristic
compounds",
which are compounds that are characteristic of the oregano plant and are
therefore indicative of
the inclusion of oregano plant particles within the aerosol-generating
substrate.
The amounts of the characteristic compounds present in pure oregano particles
are
expected to be different from the amounts that are present in the aerosol-
generating substrate.
The process of making the substrate, which involves hydration in a slurry or
suspension, and
drying at elevated temperatures, as well as the presence of other ingredients,
such as aerosol
former, will differentially modify the amounts of each of the characteristic
compounds. The
integrity of the oregano particles and the stability of a compound, under the
temperature and
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subject to the manipulations during the manufacturing will also affect the
final amount of the
compound that is present in a substrate. It is therefore contemplated that the
ratio of the
characteristic compounds relative to each other would be different after the
oregano particles
are incorporated into a substrate in various physical forms, e.g., sheets,
strands and granules.
The presence of oregano within an aerosol-generating substrate and the
proportion of
oregano provided within an aerosol-generating substrate can be determined by
measuring the
amount of the characteristic compounds within the substrate and comparing this
to the
corresponding amount of the characteristic compound in pure oregano material.
The presence
and amount of the characteristic compounds can be conducted using any suitable
techniques,
which would be known to the skilled person.
In a suitable technique, a sample of 250 milligrams of the aerosol-generating
substrate is
mixed with 5 millilitres of methanol and extracted by shaking, vortexing for 5
minutes and
centrifuging (4500 g, 5 minutes, 10 degrees Celsius). Aliquots (300
microlitres) of the extract
are transferred into a silanized chromatographic vial and diluted with
methanol (600 microlitres)
and internal standard (ISTD) solution (100 microlitres). The vials are closed
and mixed for 5
minutes using an Eppendorf ThermoMixer (5 degrees Celsius; 2000 rpm). Test
samples from
the resultant extract are analysed by LC-HRAM-MS in combined full scan mode
and data
dependent fragmentation mode for identification of the characteristic
compounds.
In some embodiments, the homogenised oregano material further comprises up to
about
75 percent by weight of tobacco particles, on a dry weight basis.
For example, the homogenised oregano material preferably comprises between
about 10
percent and about 75 percent by weight tobacco particles, more preferably
between about 15
percent and about 70 percent by weight tobacco particles, more preferably
between about 20
percent and about 65 percent by weight tobacco particles, more preferably
between about 25
percent and about 60 percent by weight tobacco particles, more preferably
between about 30
percent and about 70 percent by weight tobacco particles, on a dry weight
basis.
In some preferred embodiments, the homogenised oregano material comprises
between
about 5 percent and about 20 percent by weight of oregano particles and
between about 55
percent and about 70 percent by weight of tobacco particles, on a dry weight
basis.
The weight ratio of the oregano particles and the tobacco particles in the
particulate plant
material forming the homogenised oregano material may vary depending on the
desired flavour
characteristics and composition of the aerosol. Preferably, the homogenised
oregano material
comprises a weight ratio of oregano particles to tobacco particles that is no
more than 1:4. This
means that the oregano particles account for no more than 20 percent of the
total particulate
plant material. More preferably the homogenised oregano material comprises a
weight ratio of
oregano particles to tobacco particles that is no more than 1:5 and more
preferably less no more
than 1:6.
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For example, in a first preferred embodiment, the ratio by weight of oregano
particles to
tobacco particles is 14. A 14 ratio corresponds to a particulate plant
material consisting of
about 20 percent by weight oregano particles and about 80 percent by weight
tobacco particles.
For homogenised oregano material formed with about 75 percent by weight of
particulate plant
material, this corresponds to about 15 percent by weight of oregano particles
and about 60
percent by weight of tobacco particles in the homogenised oregano material,
based on dry
weight.
In another embodiment, the homogenised oregano material comprises a 1:9 weight
ratio
of oregano particles to tobacco particles. In yet another embodiment, the
homogenised oregano
material comprises a 1:30 weight ratio of oregano particles to tobacco
particles.
With reference to the present invention, the term "tobacco particles"
describes particles of
any plant member of the genus Nicotiana. The term "tobacco particles"
encompasses ground
or powdered tobacco leaf lamina, ground or powdered tobacco leaf stems,
tobacco dust,
tobacco fines, and other particulate tobacco by-products formed during the
treating, handling
and shipping of tobacco. In a preferred embodiment, the tobacco particles are
substantially all
derived from tobacco leaf lamina. By contrast, isolated nicotine and nicotine
salts are
compounds derived from tobacco but are not considered tobacco particles for
purposes of the
invention and are not included in the percentage of particulate plant
material.
The tobacco particles may be prepared from one or more varieties of tobacco
plants. Any
type of tobacco may be used in a blend. Examples of tobacco types that may be
used include,
but are not limited to, sun-cured tobacco, flue-cured tobacco, Burley tobacco,
Maryland tobacco,
Oriental tobacco, Virginia tobacco, and other speciality tobaccos.
Flue-curing is a method of curing tobacco, which is particularly used with
Virginia
tobaccos. During the flue-curing process, heated air is circulated through
densely packed
tobacco. During a first stage, the tobacco leaves turn yellow and wilt. During
a second stage,
the laminae of the leaves are completely dried. During a third stage, the leaf
stems are
completely dried.
Burley tobacco plays a significant role in many tobacco blends. Burley tobacco
has a
distinctive flavour and aroma and also has an ability to absorb large amounts
of casing.
Oriental is a type of tobacco which has small leaves, and high aromatic
qualities. However,
Oriental tobacco has a milder flavour than, for example, Burley. Generally,
therefore, Oriental
tobacco is used in relatively small proportions in tobacco blends.
Kasturi, Madura and Jatim are subtypes of sun-cured tobacco that can be used.
Preferably, Kasturi tobacco and flue-cured tobacco may be used in a blend to
produce the
tobacco particles. Accordingly, the tobacco particles in the particulate plant
material may
comprise a blend of Kasturi tobacco and flue-cured tobacco.
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The tobacco particles may have a nicotine content of at least about 2.5
percent by weight,
based on dry weight. More preferably, the tobacco particles may have a
nicotine content of at
least about 3 percent, even more preferably at least about 3.2 percent, even
more preferably at
least about 3.5 percent, most preferably at least about 4 percent by weight,
based on dry weight.
When the aerosol-generating substrate contains tobacco particles in
combination with oregano
particles, tobaccos having a higher nicotine content are preferred to maintain
similar levels of
nicotine relative to typical aerosol-generating substrates without oregano
particles, since the
total amount of nicotine would otherwise be reduced due to substitution of
tobacco particles with
oregano particles.
Alternatively, the tobacco particles may have a nicotine content of less than
about 2.5
percent by weight, based on dry weight. For example, the tobacco particles may
have a nicotine
content of less than about 2 percent by weight, or less than about 1.5 percent
by weight, or less
than about 1 percent by weight, based on dry weight. In some embodiments, the
tobacco
particles may have a nicotine level of substantially zero.
As a result of the inclusion of the tobacco particles, the aerosol-generating
substrate and
the aerosol generated from the aerosol-generating substrate of such
embodiments comprise
certain proportions of the "characteristic compounds" of tobacco.
Characteristic compounds
generated from tobacco include but are not limited to anatabine, cotinine, and
damascenone.
Nicotine may optionally be incorporated into the aerosol-generating substrate
although
this would be considered as a non-tobacco material for the purposes of the
invention. The
nicotine may comprise one or more nicotine salts selected from the list
consisting of nicotine
lactate, nicotine citrate, nicotine pyruvate, nicotine bitartrate, nicotine
benzoate, nicotine pectate,
nicotine alginate, and nicotine salicylate. Nicotine may be incorporated in
addition to a tobacco
with low nicotine content, or nicotine may be incorporated into an aerosol-
generating substrate
that has a reduced or zero tobacco content.
In certain embodiments of the invention, the aerosol-generating substrate
comprises a
homogenised oregano material formed from particulate plant material consisting
of oregano
particles only, with nicotine, such as a nicotine salt, incorporated into the
aerosol-generating
substrate.
Preferably, the aerosol-generating substrate comprises at least about 0.1 mg
of nicotine
per gram of the substrate, on a dry weight basis. More preferably, the aerosol-
generating
substrate comprise at least about 0.5 mg of nicotine per gram of the
substrate, more preferably
at least about 1 mg of nicotine per gram of the substrate, more preferably at
least about 1.5 mg
of nicotine per gram of the substrate, more preferably at least about 2 mg of
nicotine per gram
of the substrate, more preferably at least about 3 mg of nicotine per gram of
the substrate, more
preferably at least about 4 mg of nicotine per gram of the substrate, more
preferably at least
about 5 mg of nicotine per gram of the substrate, on a dry weight basis.
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Preferably, the aerosol-generating substrate comprises up to about 50 mg of
nicotine per
gram of the substrate, on a dry weight basis. More preferably, the aerosol-
generating substrate
comprises up to about 45 mg of nicotine per gram of the substrate, more
preferably up to about
40 mg of nicotine per gram of the substrate, more preferably up to about 35 mg
of nicotine per
gram of the substrate, more preferably up to about 30 mg of nicotine per gram
of the substrate,
more preferably up to about 25 mg of nicotine per gram of the substrate, more
preferably up to
about 20 mg of nicotine per gram of the substrate, on a dry weight basis.
For example, the aerosol-generating substrate may comprise between about 0.1
mg and
about 50 mg of nicotine per gram of the substrate, or between about 0.5 mg and
about 45 mg
of nicotine per gram of the substrate, or between about 1 mg and about 40 mg
of nicotine per
gram of the substrate, or between about 2 mg and about 35 mg of nicotine per
gram of the
substrate, or between about 5 mg and about 30 mg of nicotine per gram of the
substrate, or
between about 10 mg and about 25 mg of nicotine per gram of the substrate, or
between about
mg and about 20 mg of nicotine per gram of the substrate, on a dry weight
basis. In certain
15 preferred embodiments of the invention, the aerosol-generating substrate
comprises between
about 1 mg and about 20 mg of nicotine per gram of the substrate, on a dry
weight basis.
The defined ranges of nicotine content for the aerosol-generating substrate
include all
forms of nicotine which may be present in the aerosol-generating substrate,
including nicotine
intrinsically present in tobacco material as well as nicotine that has been
optionally added
separately to the aerosol-generating substrate, for example, in the form of a
nicotine salt.
In some embodiments, the aerosol-generating substrate comprises substantially
zero
nicotine.
Alternatively or in addition to the inclusion of tobacco particles into the
homogenised
oregano material of the aerosol-generating substrate according to the
invention, the
homogenised oregano material may comprise up to 75 percent by weight of
cannabis particles,
on a dry weight basis. The term "cannabis particles" refers to particles of a
cannabis plant, such
as the species Cannabis sativa, Cannabis indica, and Cannabis ruderalis.
For example, the particulate plant material may comprises between about 40
percent and
about 75 percent by weight of cannabis particles, more preferably between
about 45 percent
and about 60 percent by weight tobacco particles, more preferably between
about 50 percent
and about 65 percent by weight tobacco particles, on a dry weight basis_
One or more cannabinoid compounds may optionally be incorporated into the
aerosol-
generating substrate although this would be considered as a non-cannabis
material for the
purposes of the invention. As used herein with reference to the invention, the
term "cannabinoid
compound" describes any one of a class of naturally occurring compounds that
are found in
parts of the cannabis plant ¨ namely the species Cannabis sativa, Cannabis
indica, and
Cannabis ruderalis. Cannabinoid compounds are especially concentrated in the
female flower
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heads and commonly sold as cannabis oil. Cannabinoid compounds naturally
occurring the in
cannabis plant include tetrahydrocannabinol (THC) and cannabidiol (CBD). In
the context of
the present invention, the term "cannabinoid compounds" is used to describe
both naturally
derived cannabinoid compounds and synthetically manufactured cannabinoid
compounds.
For example, the aerosol-generating substrate may comprise a cannabinoid
compound
selected from the group consisting of: tetrahydrocannabinol (THC),
tetrahydrocannabinolic acid
(THCA), cannabidiol (CBD), cannabidiolic acid (CBDA), cannabinol (CBN),
cannabigerol
(CBG), cannabigerol monomethyl ether (CBGM), cannabivarin (CBV),
cannabidivarin (CBDV),
tetrahydrocannabivarin (THCV), cannabichromene (CBC), cannabicyclol (CBL),
cannabichromevarin (CBCV), cannabigerovarin (CBGV), cannabielsoin (CBE),
cannabicitran
(CBT) and combinations thereof.
The homogenised oregano material may further comprise a proportion of other
plant
flavour particles in addition to the oregano particles or the combination of
oregano particles with
at least one of tobacco particles and cannabis particles (the "particulate
plant material").
For the purposes of the present invention, the term "other plant flavour
particles" refers to
particles of non-oregano, non-tobacco and non-cannabis plant material, that
are capable of
generating one or more flavorants upon heating. This term should be considered
to exclude
particles of inert plant material such as cellulose, that do not contribute to
the sensory output of
the aerosol-generating substrate. The particles may be derived from ground or
powdered leaf
lamina, fruits, stalks, stems, roots, seeds, buds or bark from the other
plants. Suitable plant
flavour particles for inclusion in an aerosol-generating substrate according
to the invention would
be known to the skilled person and include but are not limited to clove
particles, tea particles,
bamboo particles, industrial hemp particles and combinations thereof.
The composition of the homogenised oregano material can advantageously be
adjusted
through the blending of desired amounts and types of the different plant
particles. This enables
an aerosol-generating substrate to be formed from a single homogenised oregano
material, if
desired, without the need for the combination or mixing of different blends,
as is the case for
example in the production of conventional cut filler. The production of the
aerosol-generating
substrate can therefore potentially be simplified.
The particulate plant material used in the aerosol-generating substrates of
the present
invention may be adapted to provide a desired particle size distribution.
Particle size
distributions herein are stated as D-values, whereby the D-value refers to the
percentage of
particles by number that has a diameter of less than or equal to the given D-
value. For instance,
in a D95 particle size distribution, 95 percent of the particles by number are
of a diameter less
than or equal to the given D95 value, and 5 percent of the particles by number
are of a diameter
measuring greater than the given D95 value. Similarly, in a 05 particle size
distribution, 5
percent of the particles by number are of a diameter less than or equal to the
D5 value, and 95
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percent of the particles by number are of a diameter greater than the given D5
value. In
combination, the D5 and D95 values therefore provide an indication of the
particle size
distribution of the particulate plant material.
The particulate plant material may have a D95 value of from greater than or
equal to 50
microns to a D95 value of less than or equal to 400 microns. By this is meant
that the particulate
plant material may be of a distribution represented by any D95 value within
the given range, that
is D95 may be equal to 50 microns, or D95 may be equal to 55 microns, et
cetera, all the way
up to D95 may be equal to 400 microns. By providing a D95 value within this
range, the inclusion
of relatively large plant particles into the homogenised oregano material is
avoided. This is
desirable, since the generation of aerosol from such large plant particles is
likely to be relatively
inefficient. Furthermore, the inclusion of large plant particles in the
homogenised oregano
material may adversely impact the consistency of the material.
Preferably the particulate plant material may have a 095 value of from greater
than or
equal to about 50 microns to a D95 value of less than or equal to about 350
microns, more
preferably a D95 value of from greater than or equal to about 75 microns to a
D95 value of less
than or equal to about 300 microns. The particulate oregano material and the
particulate
tobacco material may both have D95 values of from greater than or equal to
about 50 microns
to D95 values of less than or equal to about 400 microns, preferably D95
values of from greater
than or equal to 75 microns to D95 values of less than or equal to about 350
microns, more
preferably D95 values of from greater than or equal to about 100 microns to
D95 values of less
than or equal to about 300 microns.
Preferably, the particulate plant material may have a D5 value of from greater
than or
equal to about 10 microns to a D5 value of less than or equal to about 50
microns, more
preferably a D5 value of from greater than or equal to about 20 microns to a
D5 value of less
than or equal to about 40 microns. By providing a D5 value within this range,
the inclusion of
very small dust particles into the homogenised oregano material is avoided,
which may be
desirable from a manufacturing point of view.
In some embodiments, the particulate plant material including the oregano
particles may
be purposely ground to form particles having the desired particle size
distribution. The use of
purposely ground plant material advantageously improves the homogeneity of the
particulate
plant material and the consistency of the homogenised oregano material.
The diameter of 100 percent of the particulate plant material may be less than
or equal
to about 300 microns, more preferably less than or equal to about 275 microns.
The diameter
of 100 percent of the particulate oregano material and 100 percent of the
particulate tobacco
material may be less than or equal to about 300 microns, more preferably less
than or equal to
about 275 microns. The particle size range of the oregano particles enables
oregano particles
to be combined with tobacco particles in existing cast leaf processes.
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The homogenised oregano material preferably comprises at least about 55
percent by
weight of the particulate plant material including oregano particles, as
described above, more
preferably at least about 60 percent by weight of the particulate plant
material and more
preferably at least about 65 percent by weight of the particulate plant
material, on a dry weight
basis. The homogenised oregano material preferably comprises no more than
about 95 percent
by weight of the particulate plant material, more preferably no more than
about 90 percent by
weight of the particulate plant material and more preferably no more than
about 85 percent by
weight of the particulate plant material, on a dry weight basis. For example,
the homogenised
oregano material may comprise between about 55 percent and about 95 percent by
weight of
the particulate plant material, or between about 60 percent and about 90
percent by weight of
the particulate plant material, or between about 65 percent and about 85
percent by weight of
the particulate plant material, on a dry weight basis. In one particularly
preferred embodiment,
the homogenised oregano material comprises about 75 percent by weight of the
particulate plant
material, on a dry weight basis.
The particulate plant material is therefore typically combined with one or
more other
components to form the homogenised oregano material.
As defined above, the homogenised oregano material further comprises an
aerosol
former. Upon volatilisation, an aerosol former can convey other vaporised
compounds released
from the aerosol-generating substrate upon heating, such as nicotine and
flavorants, in an
aerosol. The aerosolisation of a specific compound from an aerosol-generating
substrate is
determined not solely by its boiling point. The quantity of a compound that is
aerosolised can
be affected by the physical form of the substrate, as well as by the other
components that are
also present in the substrate. The stability of a compound under the
temperature and time frame
of aerosolisation will also affect the amount of the compound that is present
in an aerosol.
Suitable aerosol formers for inclusion in the homogenised oregano material are
known in
the art and include, but are not limited to: polyhydric alcohols, such as
triethylene glycol,
propylene glycol, 1,3-butanediol and glycerol; esters of polyhydric alcohols,
such as glycerol
mono-, di- or triacetate; and aliphatic esters of mono-, di- or polycarboxylic
acids, such as
di methyl dodecanedioate and dimethyl tetradecanedioate. The homogenised
oregano material
may comprise a single aerosol former, or a combination of two or more aerosol
formers.
The homogenised oregano material preferably has an aerosol former content of
between
about 5 percent and about 30 percent by weight on a dry weight basis, such as
between about
10 percent and about 25 percent by weight on a dry weight basis, or between
about 15 percent
and about 20 percent by weight on a dry weight basis.
For example, if the substrate is intended for use in an aerosol-generating
article for an
electrically-operated aerosol-generating system having a heating element, it
may preferably
include an aerosol former content of between about 5 percent to about 30
percent by weight on
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a dry weight basis. If the substrate is intended for use in an aerosol-
generating article for an
electrically-operated aerosol-generating system having a heating element, the
aerosol former is
preferably glycerol.
In other embodiments, the homogenised oregano material may have an aerosol
former
content of about 1 percent to about 5 percent by weight on a dry weight basis.
For example, if
the substrate is intended for use in an aerosol-generating article in which
aerosol former is kept
in a reservoir separate from the substrate, the substrate may have an aerosol
former content of
greater than 1 percent and less than about 5 percent. In such embodiments, the
aerosol former
is volatilised upon heating and a stream of the aerosol former is contacted
with the aerosol-
generating substrate so as to entrain the flavours from the aerosol-generating
substrate in the
aerosol.
The aerosol former may act as a humectant in the aerosol-generating substrate.
Alternatively or in addition, the homogenised oregano material may further
comprise an
acid. The acid may comprise a carboxylic acid. The carboxylic acid may include
a ketone group.
Preferably the carboxylic acid may include a ketone group having less than
about 10 carbon
atoms, or less than about 6 carbon atoms or less than about 4 carbon atoms,
such as levulinic
acid or lactic acid. The inclusion of an acid may be particularly advantageous
where the aerosol-
generating substrate is in the form of a gel, as described below.
As defined above, the homogenised oregano material further comprises a binder
to alter
the mechanical properties of the particulate plant material, wherein the
binder is included in the
homogenised oregano material during manufacturing as described herein.
Suitable exogenous
binders would be known to the skilled person and include but are not limited
to: gums such as,
for example, guar gum, xanthan gum, arabic gum and locust bean gum; cellulosic
binders such
as, for example, hydroxypropyl cellulose, carboxymethyl cellulose,
hydroxyethyl cellulose,
methyl cellulose and ethyl cellulose; polysaccharides such as, for example,
starches, organic
acids, such as alginic acid, conjugate base salts of organic acids, such as
sodium-alginate, agar
and pectins; and combinations thereof. Preferably, the binder comprises guar
gum.
Preferably, the binder is present in an amount of from about 1 percent to
about 10 percent
by weight, based on the dry weight of the homogenised oregano material,
preferably in an
amount of from about 2 percent to about 5 percent by weight, based on the dry
weight of the
homogenised oregano material.
In addition, the homogenised oregano material may optionally further comprise
one or
more lipids to facilitate the diffusivity of volatile components (for example,
aerosol formers, (E)-
anethole and nicotine), wherein the lipid is included in the homogenised
oregano material during
manufacturing as described herein. Suitable lipids for inclusion in the
homogenised plant
material include, but are not limited to: medium-chain triglycerides, cocoa
butter, palm oil, palm
kernel oil, mango oil, shea butter, soybean oil, cottonseed oil, coconut oil,
hydrogenated coconut
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oil, candellila wax, carnauba wax, shellac, sunflower wax, sunflower oil, rice
bran, and Revel A;
and combinations thereof.
Alternatively or in addition, the homogenised oregano material may further
comprise a
pH modifier.
Alternatively or in addition, the homogenised oregano material may further
comprise
reinforcement fibers to alter the mechanical properties of the homogenised
oregano material,
wherein the reinforcement fibers are included in the homogenised oregano
material during
manufacturing as described herein. Suitable exogenous fibers for inclusion in
the homogenised
oregano material are known in the art and include fibers formed from non-
tobacco material and
non-oregano material, including but not limited to: cellulose fibers; soft-
wood fibers; hard-wood
fibers; jute fibers and combinations thereof. Exogenous fibers derived from
tobacco and/or
oregano can also be added. Any fibers added to the homogenised oregano
material are not
considered to form part of the "particulate plant material" as defined above.
Prior to inclusion in
the homogenised oregano material, fibers may be treated by suitable processes
known in the
art including, but not limited to: mechanical pulping; refining; chemical
pulping; bleaching;
sulphate pulping; and combinations thereof. A fiber typically has a length
greater than its width.
Suitable fibers typically have lengths of greater than 400 micrometres and
less than or
equal to 4 mm, preferably within the range of 0.7 mm to 4 mm. Preferably, the
fibers are present
in an amount of at least about 2 percent by weight, based on the dry weight of
the substrate.
The amount of fibers in the homogenised oregano material may depend upon the
type of
material and in particular, the method that is used to produce the homogenised
oregano
material. In some embodiments, the fibers may be present in an amount of
between about 2
percent by weight and about 15 percent by weight, most preferably at about 4
percent by weight,
based on the dry weight of the substrate. For example, this level of fibers
may be present where
the homogenised plant material is in the form of cast leaf. In other
embodiments, the fibers may
be present in an amount of at least about 30 percent by weight, or at least
about 40 percent by
weight. For example, this higher level of fibers is likely to be provided
where the homogenised
oregano material is a oregano paper formed in a papermaking process.
In preferred embodiments of the invention, the homogenised oregano material
comprises
oregano particles, between about 5 percent by weight and about 30 percent by
weight of aerosol
former and between about 1 percent by weight and about 10 percent by weight of
binder, on a
dry weight basis. In such embodiments, the homogenised oregano material
preferably further
comprises between about 2 percent by weight and about 15 percent by weight of
fibers.
Particularly preferably, the binder is guar gum.
The homogenised plant material of the aerosol-generating substrate according
to the
invention may comprises a single type of homogenised plant material or two or
more types of
homogenised plant material having a different composition or form to each
other. For example,
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in one embodiment, the aerosol-generating substrate comprises oregano
particles and tobacco
particles or cannabis particles contained within the same sheet of homogenised
plant material.
However, in other embodiments, the aerosol-generating substrate may comprise
tobacco
particles or cannabis particles and oregano particles within different sheets
to each other.
The homogenised oregano material is preferably in the form of a solid or a
gel. However,
in some embodiments the homogenised material may be in the form of a solid
that is not a gel.
Preferably, the homogenised material is not in the form of a film.
The homogenised plant material can be provided in any suitable form. For
example, the
homogenised oregano material may be in the form of one or more sheets. As used
herein with
reference to the invention, the term "sheet" describes a laminar element
having a width and
length substantially greater than the thickness thereof.
Alternatively or in addition, the homogenised oregano material may be in the
form of a
plurality of pellets or granules.
Alternatively or in addition, the homogenised oregano material may be in a
form that can
fill a cartridge or a shisha consumable, or that can be used in a shisha
device. The invention
includes a cartridge or a shisha device that contains a homogenised oregano
material.
Alternatively or in addition, the homogenised oregano material may be in the
form of a
plurality of strands, strips or shreds. As used herein, the term "strand"
describes an elongate
element of material having a length that is substantially greater than the
width and thickness
thereof. The term "strand" should be considered to encompass strips, shreds
and any other
homogenised oregano material having a similar form. The strands of homogenised
oregano
material may be formed from a sheet of homogenised oregano material, for
example by cutting
or shredding, or by other methods, for example, by an extrusion method.
In some embodiments, the strands may be formed in situ within the aerosol-
generating
substrate as a result of the splitting or cracking of a sheet of homogenised
oregano material
during formation of the aerosol-generating substrate, for example, as a result
of crimping. The
strands of homogenised oregano material within the aerosol-generating
substrate may be
separate from each other. Alternatively, each strand of homogenised oregano
material within
the aerosol-generating substrate may be at least partially connected to an
adjacent strand or
strands along the length of the strands. For example, adjacent strands may be
connected by
one or more fibers. This may occur, for example, where the strands have been
formed due to
the splitting of a sheet of homogenised oregano material during production of
the aerosol-
generating substrate, as described above.
Preferably, the aerosol-generating substrate is in the form of one or more
sheets of
homogenised oregano material. In various embodiments of the invention, the one
or more
sheets of homogenised oregano material may be produced by a casting process.
In various
embodiments of the invention, the one or more sheets of homogenised oregano
material may
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be produced by a paper-making process. The one or more sheets as described
herein may
each individually have a thickness of between 100 micrometres and 600
micrometres, preferably
between 150 micrometres and 350 micrometres, and most preferably between 200
micrometres
and 250 micrometres. Individual thickness refers to the thickness of the
individual sheet,
whereas combined thickness refers to the total thickness of all sheets that
make up the aerosol-
generating substrate. For example, if the aerosol-generating substrate is
formed from two
individual sheets, then the combined thickness is the sum of the thickness of
the two individual
sheets or the measured thickness of the two sheets where the two sheets are
stacked in the
aerosol-generating substrate.
The one or more sheets as described herein may each individually have a
grammage of
between about 100 g/m2 and about 300 g/m2.
The one or more sheets as described herein may each individually have a
density of from
about 0.3 g/cm3 to about 1.3 g/cm3, and preferably from about 0.7 g/cm3 to
about 1.0 g/cm3.
The term "tensile strength" is used throughout the specification to indicate a
measure of
the force required to stretch a sheet of homogenised oregano material until it
breaks. More
specifically, the tensile strength is the maximum tensile force per unit width
that the sheet
material will withstand before breaking and is measured in the machine
direction or cross
direction of the sheet material. It is expressed in units of Newtons per meter
of material (N/m).
Tests for measuring the tensile strength of a sheet material are well known. A
suitable test is
described in the 2014 publication of the International Standard ISO 1924-2
entitled "Paper and
Board ¨ Determination of Tensile Properties ¨ Part 2: Constant Rate of
Elongation Method".
The materials and equipment required to conduct a test according to ISO 1924-2
are: a
universal tensile/compression testing machine, Instron 5566, or equivalent; a
tension load cell
of 100 Newtons, Instron, or equivalent; two pneumatic action grips; a steel
gauge block of 180
0.25 millimetres length (width: about 10 millimetres, thickness: about 3
millimetres); a double-
bladed strip cutter, size 15 0.05 x about 250 millimetres, Adamel Lhomargy,
or equivalent; a
scalpel; a computer running acquisition software, Merlin, or equivalent; and
compressed air.
The sample is prepared by first conditioning the sheet of homogenised oregano
material for at least 24 hours at 22 2 degrees Celsius and 60 5% relative
humidity before
testing. A machine-direction or cross-direction sample is then cut to about
250 x 15 0.1
millimetres with the double-bladed strip cutter. The edges of the test pieces
must be cut
cleanly, so no more than three test specimens are cut at the same time.
The tensile/compression testing instrument is set up by installing the tension
load cell of
100 Newtons, switching on the Universal Tensile/Compression Testing Machine
and the
computer, and selecting the measurement method predefined in the software,
with a test speed
set to 8 millimetres per minute. The tension load cell is then calibrated and
the pneumatic action
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grips are installed. The test distance between the pneumatic action grips is
adjusted to 180
0.5 millimetres by means of the steel gauge block, and the distance and force
are set to zero.
The test specimen is then placed straight and centrally between the grips, and
touching
the area to be tested with fingers is avoided. The upper grip is closed and
the paper strip hangs
in the opened lower grip. The force is set to zero. The paper strip is then
pulled lightly down
and the lower grip is closed; the starting force must be between 0.05 and 0.20
Newtons. While
the upper grip is moving upward, a gradually increasing force is applied until
the test specimen
breaks. The same procedure is repeated with the remaining test specimens. The
result is valid
when the test specimen breaks when the grips move apart by a distance of more
than 10
millimetres. If it is not the case, the result is rejected and an additional
measurement is
performed.
VVhere the test specimen of homogenised oregano material that is available is
smaller
than the described sample in the test according to ISO 1924-2, as set out
above, the test can
readily be scaled down to accommodate the available size of test specimen.
The one or more sheets of homogenised oregano material as described herein may
each
individually have a tensile strength at peak in a cross direction of from 50
N/m to 400 N/m or
preferably from 150 N/m to 350 N/m. Given that the sheet thickness affects the
tensile strength,
and where a batch of sheets exhibits variation in thickness, it may be
desirable to normalize the
value to a specific sheet thickness.
The one or more sheets as described herein may each individually have a
tensile strength
at peak in a machine direction of from 100 N/m to 800 N/m or preferably from
280 N/m to 620
N/m, normalized to a sheet thickness of 215 pm. The machine direction refers
to the direction
in which the sheet material would be rolled onto or unrolled from a bobbin and
fed into a
machine, while the cross direction is perpendicular to the machine direction.
Such values of
tensile strength make the sheets and methods described herein particularly
suitable for
subsequent operations involving mechanical stresses.
The provision of a sheet having the levels of thickness, grammage and tensile
strength
as defined above advantageously optimises the machinability of the sheet to
form the aerosol-
generating substrate and ensures that damage, such as tearing of the sheet, is
avoided during
high speed processing of the sheet.
In embodiments of the present invention in which the aerosol-generating
substrate
comprises one or more sheets of homogenised oregano material, the sheets are
preferably in
the form of one or more gathered sheets. As used herein, the term "gathered"
denotes that the
sheet of homogenised oregano material is convoluted, folded, or otherwise
compressed or
constricted substantially transversely to the cylindrical axis of a plug or a
rod. The step of
"gathering" the sheet may be carried out by any suitable means which provides
the necessary
transverse compression of the sheet.
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As used herein, the term "longitudinal" refers to the direction corresponding
to the main
longitudinal axis of the aerosol-generating article, which extends between the
upstream and
downstream ends of the aerosol-generating article. During use, air is drawn
through the aerosol-
generating article in the longitudinal direction. The term "transverse" refers
to the direction that
is perpendicular to the longitudinal axis. As used herein, the term "length"
refers to the
dimension of a component in the longitudinal direction and the term "width"
refers to the
dimension of a component in the transverse direction. For example, in the case
of a plug or rod
having a circular cross-section, the maximum width corresponds to the diameter
of the circle.
As used herein, the term "plug" denotes a generally cylindrical element having
a
substantially polygonal, circular, oval or elliptical cross-section. As used
herein, the term "rod"
refers to a generally cylindrical element of substantially polygonal cross-
section and preferably
of circular, oval or elliptical cross-section. A rod may have a length greater
than or equal to the
length of a plug. Typically, a rod has a length that is greater than the
length of a plug. A rod
may comprise one or more plugs, preferably aligned longitudinally.
As used herein, the terms "upstream" and "downstream" describe the relative
positions of
elements, or portions of elements, of the aerosol-generating article in
relation to the direction in
which the aerosol is transported through the aerosol-generating article during
use. The
downstream end of the airflow path is the end at which aerosol is delivered to
a user of the
article.
The one or more sheets of homogenised oregano material may be gathered
transversely
relative to the longitudinal axis thereof and circumscribed with a wrapper to
form a continuous
rod or a plug. The continuous rod may be severed into a plurality of discrete
rods or plugs. The
wrapper may be a paper wrapper or a non-paper wrapper, as described in more
detail below.
Alternatively, the one or more sheets of homogenised oregano material may be
cut into
strands as referred to above. In such embodiments, the aerosol-generating
substrate comprises
a plurality of strands of the homogenised oregano material. The strands may be
used to form a
plug. Typically, the width of such strands is at least about 0.2 mm, or at
least about 0.5 mm.
Preferably, the width of such strands is no more than about 5 mm, or about
4mm, or about 3
mm, or about 1.5 mm. For example, the width of the strands may be between
about 0.25 mm
and about 5 mm, or between about 0.25 mm and about 3 mm, or between about 0.5
mm and
about 1.5 mm.
The length of the strands is preferably greater than about 5 mm, for example,
between
about 5 mm to about 20 mm, or between about 8 mm to about 15 mm, or about 12
mm.
Preferably, the strands have substantially the same length as each other. The
length of the
strands may be determined by the manufacturing process whereby a rod is cut
into shorter plugs
and the length of the strands corresponds to the length of the plug. The
strands may be fragile
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which may result in breakage especially during transit. In such cases, the
length of some of the
strands may be less than the length of the plug.
The plurality of strands preferably extend substantially longitudinally along
the length of
the aerosol-generating substrate, aligned with the longitudinal axis.
Preferably, the plurality of
strands are therefore aligned substantially parallel to each other. The
plurality of longitudinal
strands of aerosol- generating material is preferably substantially non-
coiled.
The strands of homogenised oregano material preferably each have a mass to
surface
area ratio of at least about 0.02 milligrams per square millimetre, more
preferably at least about
0.05 milligrams per square millimetre. Preferably the strands of homogenised
oregano material
each have a mass to surface area ratio of no more than about 0.2 milligrams
per square
millimetre, more preferably no more than about 0.15 milligrams per square
millimetre. The mass
to surface area ratio is calculated by dividing the mass of the strand of
homogenised oregano
material in milligrams by the geometric surface area of the strand of
homogenised oregano
material in square millimetres.
The one or more sheets of homogenised oregano material may be textured through
crimping, embossing, or perforating. The one or more sheets may be textured
prior to gathering
or prior to being cut into strands. Preferably, the one or more sheets of
homogenised oregano
material are crimped prior to gathering, such that the homogenised oregano
material may be in
the form of a crimped sheet, more preferably in the form of a gathered crimped
sheet. As used
herein, the term "crimped sheet" denotes a sheet having a plurality of
substantially parallel ridges
or corrugations usually aligned with the longitudinal axis of the article.
In one embodiment, the aerosol-generating substrate may be in the form of a
single plug
of aerosol-generating substrate. Preferably, the plug of aerosol-generating
substrate may
comprise a plurality of strands of homogenised oregano material. Most
preferably, the plug of
aerosol-generating substrate may comprise one or more sheets of homogenised
oregano
material. Preferably, the one or more sheets of homogenised oregano material
may be crimped
such that it has a plurality of ridges or corrugations substantially parallel
to the cylindrical axis of
the plug. This treatment advantageously facilitates gathering of the crimped
sheet of
homogenised oregano material to form the plug. Preferably, the one or more
sheets of
homogenised oregano material may be gathered. It will be appreciated that
crimped sheets of
homogenised oregano material may alternatively or in addition have a plurality
of substantially
parallel ridges or corrugations disposed at an acute or obtuse angle to the
cylindrical axis of the
plug. The sheet may be crimped to such an extent that the integrity of the
sheet becomes
disrupted at the plurality of parallel ridges or corrugations causing
separation of the material,
and results in the formation of shreds, strands or strips of homogenised
oregano material.
In another embodiment of the aerosol-generating substrate, the homogenised
plant
material comprises a first plug comprising a first homogenised plant material
and a second plug
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comprising a second homogenised plant material, wherein the first homogenised
plant material
and the second homogenised plant material comprise different levels of oregano
particles and
tobacco particles. For example, the first homogenised plant material may
comprise between
about 50 percent and about 75 percent by weight of oregano particles on a dry
weight basis;
and the second homogenised plant material comprises between about 50 percent
and about 75
percent by weight of tobacco particles, on a dry weight basis. Overall, in
accordance with the
invention, the homogenised plant materials within the aerosol-generating
substrate preferably
comprise at least 2.5 percent by weight of oregano particles and up to 70
percent by weight of
tobacco particles, on a dry weight basis.
In such arrangements, the first homogenised plant material preferably
comprises a first
particulate plant material with a higher proportion of oregano particles than
the second
homogenised plant material. The second homogenised plant material may be a
homogenised
tobacco material, with substantially no oregano particles.
Preferably, the first homogenised plant material may be in the form of one or
more sheets
and the second homogenised plant material may be in the form of one or more
sheets.
Optionally, the aerosol-generating substrate may comprise one or more plugs.
Preferably, the substrate may comprise a first plug and a second plug, wherein
the first
homogenised plant material may be located in the first plug and the second
homogenised plant
material may be located in the second plug.
Two or more plugs may be combined in an abutting end-to-end relationship and
extend to
form a rod. Two plugs may be placed longitudinally with a gap between them,
thereby creating
a cavity within a rod. The plugs may be in any suitable arrangement within the
rod.
For instance, in a preferred arrangement, a downstream plug comprising a major
proportion of oregano particles may abut an upstream plug comprising a major
proportion of
tobacco particles to form the rod. The alternative configuration in which the
upstream and
downstream positions of the respective plugs are changed relative to one
another is also
envisaged. Alternative configurations in which a third homogenised plant
material containing a
different proportion of oregano particles and tobacco particles and forming a
third plug are also
envisaged. VVhere two or more plugs are provided, the homogenised plant
material may be
provided in the same form in each plug or in a different form in each plug,
that is, gathered or
shredded. The one or more plugs may optionally be wrapped individually or
together in a
thermally conductive sheet material, as described below.
The first plug may comprise one or more sheets of the first homogenised plant
material,
and the second plug may comprise one or more sheets of the second homogenised
plant
material. The sum of the length of the plugs may be between about 10 mm and
about 40 mm,
preferably between about 10 and about 15 mm, more preferably about 12 mm. The
first plug
and the second plug may be of the same length or may have different lengths.
If the first plug
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and the second plug have the same lengths, the length of each plug may be
preferably from
about 6 mm to about 20 mm. Preferably, the second plug may be longer than the
first plug in
order to provide a desired ratio of tobacco particles to oregano particles in
the substrate. Overall,
preferably the substrate contains between 0 and 75 percent by weight of
tobacco particles and
between 0.5 and 75 percent by weight of oregano particles, on a dry weight
basis. Preferably
the second plug is at least 40 percent to 50 percent longer than the first
plug.
If the first homogenised plant material and the second homogenised plant
material are in
the form of one or more sheets, preferably the one or more sheets of the first
homogenised plant
material and second homogenised plant material may be gathered sheets.
Preferably the one
or more sheets of the first homogenised plant material and second homogenised
plant material
may be crimped sheets. It will be appreciated that all other physical
properties described with
reference to an embodiment in which a single homogenised plant material is
present are equally
applicable to an embodiment in which a first homogenised plant material and a
second
homogenised plant material are present. Further, it will be appreciated that
the description of
additives (such as binders, lipids, fibers, aerosol formers, humectants,
plasticisers, flavorants,
fillers, aqueous and non-aqueous solvents and combinations thereof) with
reference to an
embodiment in which a single homogenised plant material is present are equally
applicable to
an embodiment in which a first homogenised plant material and a second
homogenised plant
material are present.
In yet another embodiment of the aerosol-generating substrate, the first
homogenised
plant material is in the form of a first sheet, the second homogenised plant
material is in the form
of a second sheet, and the second sheet at least partially overlies the first
sheet.
The first sheet may be a textured sheet and the second sheet may be non-
textured.
Both the first and second sheets may be textured sheets.
The first sheet may be a textured sheet that is textured in a different way to
the second
sheet. For example, the first sheet may be crimped and the second sheet may be
perforated.
Alternatively, the first sheet may be perforated and the second sheet may be
crimped.
Both the first and second sheets may be crimped sheets that are
morphologically
different from each other. For example, the second sheet may be crimped with a
different
number of crimps per unit width of sheet compared to the first sheet.
The sheets may be gathered to form a plug. The sheets that are gathered
together to
form the plug may have different physical dimensions. The width and thickness
of the sheets
may be varied.
It may be desirable to gather together two sheets each having a different
thickness or each
having a different width. This may alter the physical properties of the plug.
This may facilitate
the formation of a blended plug of aerosol-generating substrate from sheets of
different chemical
composition.
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The first sheet may have a first thickness and the second sheet may have a
second
thickness that is a multiple of the first thickness, for example the second
sheet may have a
thickness two or three times the first thickness.
The first sheet may have a first width and the second sheet may have a second
width that
is different to the first width.
The first sheet and the second sheet may be disposed in overlapping
relationship prior to
being gathered together, or at the point at which they are gathered together.
The sheets may
have the same width and thickness. The sheets may have different thicknesses.
The sheets
may have different widths. The sheets may be differently textured.
Where it is desired that the first sheet and the second sheet are both
textured, the sheets
may be simultaneously textured prior to being gathered. For example, the
sheets may be
brought into overlapping relationship and passed through a texturing means,
such as a pair of
crimping rollers. A suitable apparatus and process for simultaneous crimping
are described with
reference to Figure 2 of WO-A-2013/178766. In a preferred embodiment, the
second sheet of
the second homogenised plant material overlies the first sheet of the first
homogenised plant
material, and the combined sheets are gathered to form a plug of aerosol-
generating substrate.
Optionally, the sheets may be crimped together prior to gathering to
facilitate gathering.
Alternatively, each sheet may be separately textured and then subsequently
brought
together to be gathered into a plug. For example, where the two sheets have a
different
thickness, it may be desirable to crimp the first sheet differently relative
to the second sheet.
It will be appreciated that all other physical properties described with
reference to an
embodiment in which a single homogenised plant material is present are equally
applicable to
an embodiment in which a first homogenised plant material and a second
homogenised plant
material are present. Further, it will be appreciated that the description of
additives (such as
binders, lipids, fibers, aerosol formers, humectants, plasticisers,
flavorants, fillers, aqueous and
non-aqueous solvents and combinations thereof) with reference to an embodiment
in which a
single homogenised plant material is present are equally applicable to an
embodiment in which
a first homogenised plant material and a second homogenised plant material are
present.
The homogenised plant material used in the aerosol-generating substrates
according to
the invention may be produced by various methods including paper making,
casting, dough
reconstitution, extrusion or any other suitable process.
Preferably, the homogenised oregano material is in the form of "cast leaf'.
The term "cast
leaf" is used herein to refer to a sheet product made by a casting process
that is based on
casting a slurry comprising plant particles (for example, oregano particles,
or tobacco particles
and oregano particles in a mixture) and a binder (for example, guar gum) onto
a supportive
surface, such as a belt conveyor, drying the slurry and removing the dried
sheet from the
supportive surface. An example of the casting or cast leaf process is
described in, for example,
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US-A-5,724,998 for making cast leaf tobacco. In a cast leaf process,
particulate plant materials
are mixed with a liquid component, typically water, to form a slurry. Other
added components
in the slurry may include fibers, a binder and an aerosol former. The
particulate plant materials
may be agglomerated in the presence of the binder. The slurry is cast onto a
supportive surface
and dried to form a sheet of homogenised oregano material.
In certain preferred embodiments, the homogenised oregano material used in
articles
according to the present invention is produced by casting. Homogenised oregano
material
made by the casting process typically comprise agglomerated particulate plant
material.
In a cast-leaf process, because substantially all the soluble fraction is kept
within the
plant material, most flavours are advantageously preserved. Additionally,
energy-intensive
paper-making steps are avoided.
In one preferred embodiment of the present invention, to form homogenised
oregano
material, a mixture comprising particulate plant material, water, a binder,
and an aerosol former
is formed. A sheet is formed from the mixture, and the sheet is then dried_
Preferably the mixture
is an aqueous mixture. As used herein, "dry weight" refers to the weight of a
particular non-
water component relative to the sum of the weights of all non-water components
in a mixture,
expressed as a percentage. The composition of aqueous mixtures may be referred
to by
"percentage dry weight." This refers to the weight of the non-water components
relative to the
weight of the entire aqueous mixture, expressed as a percentage.
The mixture may be a slurry. As used herein, a "slurry" is a homogenised
aqueous mixture
with a relatively low dry weight. A slurry as used in the method herein may
preferably have a
dry weight of between 5 percent and 60 percent.
Alternatively, the mixture may be a dough. As used herein, a "dough" is an
aqueous
mixture with a relatively high dry weight. A dough as used in the method
herein may preferably
have a dry weight of at least 60 percent, more preferably at least 70 percent.
Slurries comprising greater than 30 percent dry weight and doughs may be
preferred in
certain embodiments of the present method.
The step of mixing the particulate plant material, water and other optional
components
may be carried out by any suitable means. For mixtures of a low viscosity,
that is, some slurries,
it is preferred that mixing is performed using a high energy mixer or a high
shear mixer. Such
mixing breaks down and distributes the various phases of the mixture
homogeneously. For
mixtures of a higher viscosity, that is, some doughs, a kneading process may
be used to
distribute the various phases of the mixture homogeneously.
Methods according to the present invention may further comprise the step of
vibrating the
mixture to distribute the various components. Vibrating the mixture, that is
for example vibrating
a tank or silo where a homogenised mixture is present, may help the
homogenization of the
mixture, particularly when the mixture is a mixture of low viscosity, that is,
some slurries. Less
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mixing time may be required to homogenize a mixture to the target value
optimal for casting if
vibrating is performed as well as mixing.
If the mixture is a slurry, a web of homogenised oregano material is
preferably formed by
a casting process comprising casting the slurry on a supportive surface, such
as a belt conveyor.
The method for production of a homogenised oregano material comprises the step
of drying
said cast web to form a sheet. The cast web may be dried at room temperature
or at an ambient
temperature of at least about 60 degrees Celsius, more preferably at least
about 80 degrees
Celsius for a suitable length of time. Preferably, the cast web is dried at an
ambient temperature
of no more than 200 degrees Celsius, more preferably no more than about 160
degrees Celsius.
For example, the cast web may be dried at a temperature of between about 60
degrees Celsius
and about 200 degrees Celsius, or between about 80 degrees Celsius and about
160 degrees
Celsius. Preferably, the moisture content of the sheet after drying is between
about 5 percent
and about 15 percent based on the total weight of the sheet. The sheet may
then be removed
from the supportive surface after drying. The cast sheet has a tensile
strength such that it can
be mechanically manipulated and wound or unwound from a bobbin without
breakage or
deformation.
If the mixture is a dough, the dough may be extruded in the form of a sheet,
strands, or
strips, prior to the step of drying the extruded mixture. Preferably, the
dough may be extruded
in the form of a sheet. The extruded mixture may be dried at room temperature
or at a
temperature of at least about 60 degrees Celsius, more preferably at least
about 80 degrees
Celsius for a suitable length of time. Preferably, the extruded mixture is
dried at an ambient
temperature of no more than 200 degrees Celsius, more preferably no more than
about 160
degrees Celsius. For example, the extruded mixture may be dried at a
temperature of between
about 60 degrees Celsius and about 200 degrees Celsius, or between about 80
degrees Celsius
and about 160 degrees Celsius. Preferably, the moisture content of the
extruded mixture after
drying is between about 5 percent and about 15 percent based on the total
weight of the sheet.
A sheet formed from dough requires less drying time and/or lower drying
temperatures as a
result of significantly lower water content relative to a web formed from a
slurry.
After the sheet has been dried, the method may optionally comprise a step of
coating a
nicotine salt, preferably along with an aerosol former, onto the sheet, as
described in the
disclosure of WO-A-2015/082652.
After the sheet has been dried, methods according to the invention may
optionally
comprise a step of cutting the sheet into strands, shreds or strips for the
formation of the aerosol-
generating substrate as described above.
The strands, shreds or strips may be brought
together to form a rod of the aerosol-generating substrate using suitable
means. In the formed
rod of aerosol-generating substrate, the strands, shreds or strips may be
substantially aligned,
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for example, in the longitudinal direction of the rod. Alternatively, the
strands, shreds or strips
may be randomly oriented in the rod.
Methods according to the present invention may optionally further comprise a
step of
winding the sheet onto a bobbin, after the drying step.
The present invention further provides an alternative paper-making method for
producing
sheets of homogenised plant material in the form of a plant "paper". Plant
paper refers to a
reconstituted plant sheet formed by a process in which a plant feedstock is
extracted with a
solvent to produce an extract of soluble plant compounds and an insoluble
residue of fibrous
plant material, and the extract is recombined with the insoluble residue. The
extract may
optionally be concentrated or further processed before being recombined with
the insoluble
residue. The insoluble residue may optionally be refined and combined with
additional plant
fibers before being recombined with the extract. In the method according to
the present
invention, the plant feedstock will comprise particles of oregano, optionally
in combination with
particles of tobacco.
In more detail, the method of producing a plant paper comprises a first step
of mixing a
plant material and water to form a dilute suspension. The dilute suspension
comprises mostly
separate cellulose fibers. The suspension has a lower viscosity and a higher
water content
than the slurry produced in the casting process. This first step may involve
soaking, optionally
in the presence of an alkali, such as sodium hydroxide, and optionally
applying heat.
The method further comprises a second step of separating the suspension into
an
insoluble portion containing the insoluble residue of fibrous plant material
and a liquid or
aqueous extract comprising soluble plant compounds. The water remaining in the
insoluble
residue of fibrous plant material may be drained through a screen, acting as a
sieve, such that
a web of randomly interwoven fibers may be laid down. Water may be further
removed from
this web by pressing with rollers, sometimes aided by suction or vacuum.
After removal of the aqueous portion and water, the insoluble residue is
formed into a
sheet. Preferably, a generally flat, uniform sheet of plant fibers is formed.
Preferably, the method further comprises the steps of concentrating the
extract of soluble
plant compounds that were removed from the sheet and adding the concentrated
extract into
the sheet of insoluble residue of fibrous plant material to form a sheet of
homogenised plant
material. Alternatively or in addition, a soluble plant substance or
concentrated plant substance
from another process can be added to the sheet. The extract or concentrated
extract may be
from another variety of the same species of plant, or from another species of
plant.
This process, as described in US-A-3,860,012, has been used with tobacco to
make
reconstituted tobacco products, also known as tobacco paper. The same process
can also be
used with one or more plants to produce a paper-like sheet material, such a
sheet of oregano
paper.
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In certain preferred embodiments, the homogenised plant material used in
articles
according to the present invention is produced by a paper-making process as
defined above. In
such embodiments, the homogenised oregano material is in the form of a oregano
paper.
Homogenised tobacco material or homogenised oregano material produced by such
a
process are referred to as tobacco paper or oregano paper. Homogenised plant
material made
by the paper-making process is distinguishable by the presence of a plurality
of fibers throughout
the material, visible by eye or under a light microscope, particularly when
the paper is wetted by
water. In contrast, homogenised plant material made by the casting process
comprises less
fibers than paper and tends to dissociate into a slurry when it is wetted.
Mixed tobacco oregano
paper refers to homogenised plant material produced by such a process using a
mixture of
tobacco and oregano materials.
In embodiments in which the aerosol-generating substrate comprises a
combination of
oregano particles and tobacco particles, the aerosol-generating substrate may
comprise one or
more sheets of oregano paper and one or more sheets of tobacco paper. The
sheets of oregano
paper and tobacco paper may be interleaved with each other or stacked prior to
being gathered
to form a rod. Optionally, the sheets may be crimped. Alternatively, the
sheets of oregano paper
and tobacco paper may be cut into strands, strips or shreds and then combined
to form a rod.
The relative amounts of tobacco and oregano in the aerosol-generating
substrate can be
adjusted by changing the respective number of tobacco and oregano sheets or
the respective
amounts of oregano and tobacco strands, strips or shreds in the rod.
For example, the number or amount of tobacco and oregano sheets or strands may
be
adjusted to provide a ratio of oregano to tobacco of about 1:4, or about 1:9
or about 1:30.
Other known processes that can be applied to producing homogenised plant
materials
are dough reconstitution processes of the type described in, for example, US-A-
3,894,544; and
extrusion processes of the type described in, for example, in GB-A-983,928.
Typically, the
densities of homogenised plant materials produced by extrusion processes and
dough
reconstitution processes are greater than the densities of the homogenised
plant materials
produced by casting processes.
In alternative embodiments of the present invention, the homogenised oregano
material
is in the form of a gel composition formed with the oregano particles, aerosol
former and binder.
Preferably, where the homogenised oregano material is in the form of a gel
composition
containing the oregano particles, the binder comprises a cellulose ether such
as carboxymethyl
cellulose. The binder may be present in an amount of between about 1 percent
and about 5
percent by weight, based on the total weight of the gel. For example, the gel
composition may
comprise between 1.5 percent by weight and 3.5 percent by weight of sodium
carboxymethyl
cellulose.
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Preferably, the gel composition comprises at least about 60 percent by weight
of aerosol
former, such as glycerin, based on the total weight of the gel. For example,
the gel composition
may comprise between 65 percent by weight and 85 percent by weight of
glycerin.
Optionally, the gel composition may further comprise an acid, such as lactic
acid. The
acid may be present in an amount of up to about 6 percent by weight, based on
the total weight
of the gel composition. Optionally, the gel composition may comprise up to
about 5 percent by
weight of nicotine, based on the total weight of the gel composition.
Optionally, the gel
composition comprises between about 10 percent by weight and about 30 percent
by weight of
water, based on the total weight of the gel composition.
In embodiments in which the homogenised oregano material is in the form of a
gel
composition, the aerosol-generating substrate preferably comprises a porous
medium loaded
with the gel composition. The term "porous" is used herein to refer to a
material that provides a
plurality of pores or openings that allow the passage of air through the
material.
The porous medium may be any suitable porous material able to hold or retain
the gel
composition. Ideally the porous medium can allow the gel composition to move
within it. In
specific embodiments the porous medium comprises natural materials, synthetic,
or semi-
synthetic, or a combination thereof. In specific embodiments the porous medium
comprises
sheet material, foam, or fibers, for example loose fibers; or a combination
thereof. In specific
embodiments the porous medium comprises a woven, non-woven, or extruded
material, or
combinations thereof. Preferably the porous medium comprises, cotton, paper,
viscose, PLA, or
cellulose acetate, of combinations thereof. Preferably the porous medium
comprises a sheet
material, for example, cotton or cellulose acetate. In a particularly
preferred embodiment, the
porous medium comprises a sheet made from cotton fibers.
The porous medium used in the present invention may be crimped or shredded. In
preferred embodiments, the porous medium is crimped. In alternative
embodiments the porous
medium comprises shredded porous medium. The crimping or shredding process can
be before
or after loading with the gel composition.
Preferably, when the homogenised oregano material is in the form of a gel
composition
loaded onto a porous medium, the aerosol-generating substrate comprises an
elongate
susceptor element extending longitudinally through the porous medium or
adjacent to the porous
medium.
Preferably, the aerosol-generating substrate of aerosol-generating articles
according to
the invention comprises at least about 200 mg of the homogenised oregano
material, more
preferably at least about 250 mg of the homogenised oregano material and more
preferably at
least about 275 mg of the homogenised oregano material.
Aerosol-generating articles according to the invention comprise a rod,
comprising the
aerosol-generating substrate in one or more plugs. The rod of aerosol-
generating substrate
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may have a length of from about 5 mm to about 120 mm. For example, the rod may
preferably
have a length of between about 10 and about 45 mm, more preferably between
about 10 mm
and 15 mm, most preferably about 12 mm. In alternative embodiments, the rod
preferably has
a length of between about 30 mm and about 45 mm, or between about 33 mm and
about 41
mm. Where the rod is formed of a single plug of aerosol-generating substrate,
the plug has the
same length as the rod.
The rod of aerosol-generating substrate may have an external diameter of
between about
5 mm and about 10 mm, depending on their intended use. For example, in some
embodiments,
the rod may have an external diameter of between about 5.5 mm and about 8 mm,
or between
about 6.5 mm and about 8 mm. The "external diameter of the rod of aerosol-
generating
substrate corresponds to the diameter of the rod including any wrappers.
The rod of aerosol-generating substrate of the aerosol-generating articles
according to the
invention is preferably circumscribed by one or more wrappers along at least a
part of its length.
The one or more wrappers may include a paper wrapper or a non-paper wrapper,
or both.
Suitable paper wrappers for use in specific embodiments of the invention are
known in the art
and include, but are not limited to: cigarette papers; and filter plug wraps.
Suitable non-paper
wrappers for use in specific embodiments of the invention are known in the art
and include, but
are not limited to sheets of homogenised tobacco materials. Homogenised
tobacco wrappers
are particularly suitable for use in embodiments wherein the aerosol-
generating substrate
comprises one or more sheets of homogenised oregano material formed of
particulate plant
material, the particulate plant material containing oregano particles in
combination with a low
percentage by weight of tobacco particles, such as from 20 percent to 0
percent by weight of
tobacco particles, based on dry weight.
In certain embodiments of the invention, the aerosol-generating substrate is
circumscribed
along at least a part of its length by a thermally conductive sheet material,
for example, a metallic
foil, such as aluminium foil or a metallised paper. The metallic foil or
metallised paper serves
the purpose of conducting heat rapidly throughout the aerosol-generating
substrate. In addition,
the metallic foil or metallised paper may serve to prevent the ignition of the
aerosol-generating
substrate in the event that the consumer attempts to light it. Furthermore,
during use, the
metallic foil or metallised paper may prevent odours produced upon heating of
the outer wrapper
from entering the aerosol generated from the aerosol-generating substrate_ For
example, this
may be a problem for aerosol-generating articles having an aerosol-generating
substrate that is
heated externally during use in order to generate an aerosol. Alternatively,
or in addition, a
metallised wrapper may be used to facilitate detection or recognition of the
aerosol-generating
article when it is inserted into an aerosol-generating device during use. The
metallic foil or
metallised paper may comprise metal particles, such as iron particles.
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The one or more wrappers circumscribing the aerosol-generating substrate
preferably
have a total thickness of between about 0.1 mm and about 0.9 mm.
The internal diameter of the rod of aerosol-generating substrate is preferably
between
about 3 mm and about 9.5 mm, more preferably between about 4 mm and about 7.5
mm, more
preferably between about 5 mm and about 7.5 mm. The "internal diameter"
corresponds to the
diameter of the rod of aerosol-generating substrate without including the
thickness of the
wrappers, but measured with the wrappers still in place. Aerosol-generating
articles according
to the invention also include but are not limited to a cartridge or a shisha
consumable.
Aerosol-generating articles according to the invention may optionally include
a support
element comprising at least one hollow tube immediately downstream of the
aerosol-generating
substrate. One function of the tube is to locate the aerosol-generating
substrate towards the
distal end of the aerosol-generating article so that it can be contacted with
a heating element.
The tube acts to prevent the aerosol-generating substrate from being forced
along the aerosol-
generating article towards other downstream elements when a heating element is
inserted into
the aerosol-generating substrate. The tube also acts as a spacer element to
separate the
downstream elements from the aerosol-generating substrate. The tube can be
made of any
material, such as cellulose acetate, a polymer, cardboard, or paper.
Alternatively or in addition, aerosol-generating articles according to the
invention optionally
comprise an aerosol-cooling element downstream of the aerosol-generating
substrate and
immediately downstream of the hollow tube forming the support element. In use,
an aerosol
formed by volatile compounds released from the aerosol-generating substrate
passes through
and is cooled by the aerosol-cooling element before being inhaled by a user.
The lower
temperature allows the vapours to condense into an aerosol. The aerosol-
cooling element may
be a hollow tube, such as a hollow cellulose acetate tube or a cardboard tube,
which can be
similar to the support element that is immediately downstream of the aerosol-
generating
substrate. The aerosol-cooling element may be a hollow tube of equal outer
diameter but smaller
or larger inner diameter than the hollow tube forming the support element. In
one embodiment,
the aerosol-cooling element wrapped in paper comprises one or more
longitudinal channels
made of any suitable material, such as a metallic foil, a paper laminated with
a foil, a polymeric
sheet preferably made of a synthetic polymer, and a substantially non-porous
paper or
cardboard. In some embodiments, the aerosol-cooling element wrapped in paper
may comprise
one or more sheets made of a material selected from the group consisting of
polyethylene (PE),
polypropylene (PP), polyvinylchloride (PVC), polyethylene terephthalate (PET),
polylactic acid
(PLA), cellulose acetate (CA), paper laminated with a polymeric sheet and
aluminium foil.
Alternatively, the aerosol-cooling element may be made of woven or non-woven
filaments of a
material selected from the group consisting of polyethylene (PE),
polypropylene (PP),
polyvinylchloride (PVC), polyethylene terephthalate (PET), polylactic acid
(PLA), and cellulose
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acetate (CA). In a preferred embodiment, the aerosol-cooling element is a
crimped and
gathered sheet of polylactic acid wrapped within a filter paper. In another
preferred embodiment,
the aerosol-cooling element comprises a longitudinal channel and is made of
woven filaments
of a synthetic polymer, such as polylactic acid filaments, which are wrapped
in paper.
One or more additional hollow tubes may be provided downstream of the aerosol-
cooling
element.
Aerosol-generating articles according to the invention may further comprise a
filter or
mouthpiece downstream of the aerosol-generating substrate and, where present,
the support
element and aerosol-cooling element. The filter may comprise one or more
filtration materials
for the removal of particulate components, gaseous components, or a
combination thereof.
Suitable filtration materials are known in the art and include, but are not
limited to: fibrous
filtration materials such as, for example, cellulose acetate tow and paper;
adsorbents such as,
for example, activated alumina, zeolites, molecular sieves and silica gel;
biodegradable
polymers including, for example, polylactic acid (PLA), Mater-Bie, hydrophobic
viscose fibers,
and bioplastics; and combinations thereof. The filter may be located at the
downstream end of
the aerosol-generating article. The filter may be a cellulose acetate filter
plug. The filter is about
7 mm in length in one embodiment, but may have a length of between about 5 mm
and about
10 mm.
Aerosol-generating articles according to the invention may comprise a mouth
end cavity
at the downstream end of the article. The mouth end cavity may be defined by
one or more
wrappers extending downstream from the filter or mouthpiece. Alternatively,
the mouth end
cavity may be defined by a separate tubular element provided at the downstream
end of the
aerosol-generating article.
Aerosol-generating articles according to the invention preferably further
comprise a
ventilation zone provided at a location along the aerosol-generating article.
For example, the
aerosol-generating article may be provided at a location along a hollow tube
provided
downstream of the aerosol-generating substrate.
Aerosol-generating articles according to the invention may optionally further
comprise an
upstream element at the upstream end of the aerosol-generating substrate. The
upstream
element may be a porous plug element, such as a plug of fibrous filtration
material such as
cellulose acetate.
In preferred embodiments of the invention, the aerosol-generating article
comprises the
aerosol-generating substrate, at least one hollow tube downstream of the
aerosol-generating
substrate and a filter downstream of the at least one hollow tube. Optionally,
the aerosol-
generating article further comprises a mouth end cavity at the downstream end
of the filter.
Preferably, a ventilation zone is provided at a location along the at least
one hollow tube.
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In a particularly preferred embodiment having this arrangement, the aerosol-
generating
article comprises an aerosol-generating substrate, an upstream element at the
upstream end of
the aerosol-generating substrate, a support element downstream of the aerosol-
generating
substrate, an aerosol-cooling element downstream of the support element and a
filter
downstream of the aerosol-cooling element. Preferably, the support element and
the aerosol-
cooling element are both in the form of a hollow tube. Preferably, the aerosol-
generating
substrate comprises an elongate susceptor element extending longitudinally
through it.
In one particularly preferred examples, the aerosol-generating substrate has a
length of
about 33 mm and an external diameter of between about 5.5 mm and 6.7 mm,
wherein the
aerosol-generating substrate comprises about 340 mg of the homogenised oregano
material in
the form of a plurality of strands, wherein the homogenised oregano material
comprises about
14 percent by weight glycerol on a dry weight basis. In this embodiment, the
aerosol-generating
article has a total length of about 74 mm and comprises a cellulose acetate
tow filter having a
length of about 10 mm, as well as a mouth end cavity defined by a hollow tube
having a length
of about 6-7 mm. The aerosol-generating article comprises a hollow tube
downstream of the
aerosol-generating substrate, wherein the hollow tube has a length of about 25
mm and is
provided with a ventilation zone.
The aerosol-generating articles according to the invention may have a total
length of at
least about 30 mm, or at least about 40 mm. The total length of the aerosol-
generating article
may be less than 90 mm, or less than about 80 mm.
In one embodiment, the aerosol-generating article has a total length of
between about 40
mm and about 50 mm, preferably about 45 mm. In another embodiment, the aerosol-
generating
article has a total length of between about 70 mm and about 90 mm, preferably
between about
80 mm and about 85 mm. in another embodiment, the aerosol-generating article
has a total
length of between about 72 mm and about 76 mm, preferably about 74 mm.
The aerosol-generating article may have an external diameter of about 5 mm to
about 8
mm, preferably between about 6 mm and about 8 mm. In one embodiment, the
aerosol-
generating article has an external diameter of about 7.3 mm.
Aerosol-generating articles according to the invention may further comprise
one or more
aerosol-modifying elements. An aerosol-modifying element may provide an
aerosol-modifying
agent. As used herein, the term aerosol-modifying agent is used to describe
any agent that, in
use, modifies one or more features or properties of aerosol passing through
the filter. Suitable
aerosol-modifying agents include, but are not limited to, agents that, in use,
impart a taste or
aroma to aerosol passing through the filter or agents that, in use, remove
flavors from the aerosol
passing through the filter.
An aerosol-modifying agent may be one or more of moisture or a liquid
flavorant. Water
or moisture may modify the sensorial experience of the user, for example by
moistening the
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generated aerosol, which may provide a cooling effect on the aerosol and may
reduce the
perception of harshness experienced by the user. An aerosol-modifying element
may be in the
form of a flavour-delivery element to deliver one or more liquid flavorants.
Alternatively, a liquid
flavorant may be added directly to the homogenised oregano material, for
example, by adding
the flavour to the slurry or feedstock during production of the homogenised
oregano material, or
by spraying the liquid flavourant onto the surface of the homogenised oregano
material.
The one or more liquid flavorants may comprise any flavour compound or
botanical extract
suitable for being releasably disposed in liquid form within the flavour-
delivery element to
enhance the taste of aerosol produced during use of the aerosol-generating
article. The
flavorants, liquid or solid, can also be disposed directly in the material
which forms the filter,
such as cellulose acetate tow. Suitable flavours or flavourings include, but
are not limited to,
menthol, mint, such as peppermint and spearmint, chocolate, liquorice, citrus
and other fruit
flavours, gamma octalactone, vanillin, ethyl vanillin, breath freshener
flavours, spice flavours
such as cinnamon, methyl salicylate, linalool, eugenol, bergamot oil, geranium
oil, lemon oil,
cannabis oil, and tobacco flavour. Other suitable flavours may include flavour
compounds
selected from the group consisting of an acid, an alcohol, an ester, an
aldehyde, a ketone, a
pyrazine, combinations or blends thereof and the like.
In certain embodiments of the invention, the aerosol-modifying agent may be an
essential
oil derived from one or more plants. For example, the homogenised oregano
material may
comprise an oregano oil, such as oregano essential oil, to further enhance the
oregano flavours
delivered to the consumer upon heating.
In certain embodiments of the invention, the aerosol-generating substrate may
comprise
a homogenised oregano material comprising particulate plant material, such as
tea particles, in
combination with oregano oil.
An aerosol-modifying agent may be an adsorbent material such as activated
carbon, which
removes certain constituents of the aerosol passing through the filter and
thereby modifies the
flavour and aroma of the aerosol.
The one or more aerosol-modifying elements may be located downstream of the
aerosol-
generating substrate or within the aerosol-generating substrate. The aerosol-
generating
substrate may comprise homogenised oregano material and an aerosol-modifying
element. In
various embodiments, the aerosol-modifying element may be placed adjacent to
the
homogenised oregano material or embedded in the homogenised oregano material.
Typically,
aerosol-modifying elements may be located downstream of the aerosol-generating
substrate,
most typically, within the aerosol-cooling element, within the filter of the
aerosol-generating
article, such as within a filter plug or within a cavity, preferably within a
cavity between filter
plugs. The one or more aerosol-modifying elements may be in the form of one or
more of a
thread, a capsule, a microcapsule, a bead or a polymer matrix material, or a
combination thereof.
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If an aerosol-modifying element is in the form of a thread, as described in WO-
A-
2011/060961, the thread may be formed from paper such as filter plug wrap, and
the thread
may be loaded with at least one aerosol-modifying agent and located within the
body of the filter.
Other materials that can be used to form a thread include cellulose acetate
and cotton.
If an aerosol-modifying element is in the form of a capsule, as described in
WO-A-
2007/010407, WO-A-2013/068100 and WO-A-2014/154887, the capsule may be a
breakable
capsule located within the filter, the inner core of the capsule containing an
aerosol-modifying
agent which may be released upon breakage of the outer shell of the capsule
when the filter is
subjected to external force. The capsule may be located within a filter plug
or within a cavity,
preferably a cavity between filter plugs.
If an aerosol-modifying element is in the form of a polymer matrix material,
the polymer
matrix material releases the flavorant when the aerosol-generating article is
heated, such as
when the polymer matrix is heated above the melting point of the polymer
matrix material as
described in WO-A-2013/034488. Typically, such polymer matrix material may be
located within
a bead within the aerosol-generating substrate. Alternatively, or in addition,
the flavorant may
be trapped within the domains of a polymer matrix material and releasable from
the polymer
matrix material upon compression of the polymer matrix material. Preferably,
the flavorant is
released upon compression of the polymer matrix material with a force of
around 15 Newtons.
Such flavour-modifying elements may provide a sustained release of the liquid
flavorant over a
range of force of at least 5 Newtons, such as between 5N and 20N, as described
in
W02013/068304. Typically, such polymer matrix material may be located within a
bead within
the filter.
The aerosol-generating article may comprise a combustible heat source and an
aerosol-
generating substrate downstream of the combustible heat source, the aerosol-
generating
substrate as described above with respect to the first aspect of the
invention.
For example, substrates as described herein may be used in heated aerosol-
generating
articles of the type disclosed in WO-A-2009/022232, which comprise a
combustible carbon-
based heat source, an aerosol-generating substrate downstream of the
combustible heat
source, and a heat-conducting element around and in contact with a rear
portion of the
combustible carbon-based heat source and an adjacent front portion of the
aerosol-generating
substrate. However, it will be appreciated that substrates as described herein
may also be used
in heated aerosol-generating articles comprising combustible heat sources
having other
constructions.
The present invention provides an aerosol-generating system comprising an
aerosol-
generating device comprising a heating element, and an aerosol-generating
article for use with
the aerosol-generating device, the aerosol-generating article comprising the
aerosol-generating
substrate as described above.
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In a preferred embodiment, aerosol-generating substrates as described herein
may be
used in heated aerosol-generating articles for use in electrically-operated
aerosol-generating
systems in which the aerosol-generating substrate of the heated aerosol-
generating article is
heated by an electrical heat source.
For example, aerosol-generating substrates as described herein may be used in
heated
aerosol-generating articles of the type disclosed in EP-A-0 822 760.
The heating element of such aerosol-generating devices may be of any suitable
form to
conduct heat. The heating of the aerosol-generating substrate may be achieved
internally,
externally or both. The heating element may preferably be a heater blade or
pin adapted to be
inserted into the substrate so that the substrate is heated from inside.
Alternatively, the heating
element may partially or completely surround the substrate and heat the
substrate
circumferentially from the outside.
The aerosol-generating system may be an electrically-operated aerosol
generating
system comprising an inductive heating device. Inductive heating devices
typically comprise an
induction source that is configured to be coupled to a susceptor, which may be
provided
externally to the aerosol-generating substrate or internally within the
aerosol-generating
substrate. The induction source generates an alternating electromagnetic field
that induces
magnetization or eddy currents in the susceptor. The susceptor may be heated
as a result of
hysteresis losses or induced eddy currents which heat the susceptor through
ohmic or resistive
heating.
Electrically operated aerosol-generating systems comprising an inductive
heating device
may also comprise the aerosol-generating article having the aerosol-generating
substrate and
a susceptor in thermal proximity to the aerosol-generating substrate.
Typically, the susceptor is
in direct contact with the aerosol-generating substrate and heat is
transferred from the susceptor
to the aerosol-generating substrate primarily by conduction. Examples of
electrically operated
aerosol-generating systems having inductive heating devices and aerosol-
generating articles
having susceptors are described in WO-A1-95/27411 and WO-A1-2015/177255.
A susceptor may be a plurality of susceptor particles which may be deposited
on or
embedded within the aerosol-generating substrate. VVhen the aerosol-generating
substrate is
in the form of one or more sheets, a plurality of susceptor particles may be
deposited on or
embedded within the one or more sheets. The susceptor particles are
immobilized by the
substrate, for example, in sheet form, and remain at an initial position.
Preferably, the susceptor
particles may be homogeneously distributed in the homogenised oregano material
of the
aerosol-generating substrate. Due to the particulate nature of the susceptor,
heat is produced
according to the distribution of the particles in the homogenised oregano
material sheet of the
substrate. Alternatively, the susceptor in the form of one or more sheets,
strips, shreds or rods
may also be placed next to the homogenised oregano material or used as
embedded in the
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homogenised oregano material. In one embodiment, the aerosol forming substrate
comprises
one or more susceptor strips. For example, the rod of aerosol-generating
substrate may
comprise an elongate susceptor element extending longitudinally through it. In
another
embodiment, the susceptor is present in the aerosol-generating device.
The susceptor may have a heat loss of more than 0.05 Joule per kilogram,
preferably a
heat loss of more than 0.1 Joule per kilogram. Heat loss is the capacity of
the susceptor to
transfer heat to the surrounding material. Because the susceptor particles are
preferably
homogeneously distributed in the aerosol-generating substrate, a uniform heat
loss from the
susceptor particles may be achieved thus generating a uniform heat
distribution in the aerosol-
generating substrate and leading to a uniform temperature distribution in the
aerosol-generating
article. It has been found that a specific minimal heat loss of 0.05 Joule per
kilogram in the
susceptor particles allows for heating of the aerosol-generating substrate to
a substantially
uniform temperature, thus providing aerosol generation. Preferably, the
average temperatures
achieved within the aerosol-generating substrate in such embodiments are about
200 degree
Celsius to about 240 degrees Celsius.
Reducing the risk of overheating the aerosol-generating substrate may be
supported by
the use of susceptor materials having a Curie temperature, which allows a
heating process due
to hysteresis loss only up to a certain maximum temperature. The susceptor may
have a Curie
temperature between about 200 degree Celsius and about 450 degree Celsius,
preferably
between about 240 degree Celsius and about 400 degree Celsius, for example
about 280
degree Celsius. VVhen a susceptor material reaches its Curie temperature, the
magnetic
properties change. At the Curie temperature the susceptor material changes
from a
ferromagnetic phase to a paramagnetic phase. At this point, heating based on
energy loss due
to orientation of ferromagnetic domains stops. Further heating is then mainly
based on eddy
current formation such that a heating process is automatically reduced upon
reaching the Curie
temperature of the susceptor material. Preferably, susceptor material and its
Curie temperature
are adapted to the composition of the aerosol-generating substrate in order to
achieve an
optimal temperature and temperature distribution in the aerosol-generating
substrate for an
optimum aerosol generation.
In some preferred embodiments of the aerosol-generating article according to
the
invention, the susceptor is made of ferrite_ Ferrite is a ferromagnet with a
high magnetic
permeability and especially suitable as susceptor material. The main component
of ferrite is iron.
Other metallic components, for example, zinc, nickel, manganese, or non-
metallic components,
for example silicon, may be present in varying amounts. Ferrite is a
relatively inexpensive,
commercially available material. Ferrite is available in particle form in the
size ranges of the
particles used in the particulate plant material forming the homogenised plant
material according
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to the invention. Preferably, the particles are a fully sintered ferrite
powder, such as for example
FP160, FP215, FP350 by PPT, Indiana USA.
In certain embodiments of the invention, the aerosol-generating system
comprises an
aerosol-generating article comprising an aerosol-generating substrate as
defined above, a
source of aerosol former and a means to vaporise the aerosol former,
preferably a heating
element as described above. The source of aerosol former can be a reservoir,
which can be
refillable or replaceable, that resides on the aerosol generating device.
While the reservoir is
physically separate from the aerosol generating article, the vapour that is
generated is directed
through the aerosol-generating article. The vapour makes contact with the
aerosol-generating
substrate which releases volatile compounds, such as nicotine and flavorants
in the particulate
plant material, to form an aerosol. Optionally, to aid volatilization of
compounds in the aerosol-
generating substrate, the aerosol-generating system may further comprise a
heating element to
heat the aerosol-generating substrate, preferably in a co-ordinated manner
with the aerosol
former. However, in certain embodiments, the heating element used to heat the
aerosol
generating article is separate from the heater that heats the aerosol former.
As defined above, the present invention further provides an aerosol produced
upon
heating of an aerosol-generating substrate, wherein the aerosol comprises
specific amounts
and ratios of the characteristic compounds derived from oregano particles as
defined above.
According to the invention, the aerosol comprises ursolic acid in an amount of
at least
0.04 micrograms per puff of aerosol; isothymol in an amount of at least 0.01
micrograms per
puff of aerosol; and thymohydroquinone in an amount of at least 0.01
micrograms per puff of
aerosol, wherein a puff of aerosol has a volume of 55 millilitres as generated
by a smoking
machine. For the purposes of the present invention, a "puff" is defined as a
volume of aerosol
released from an aerosol-generating substrate upon heating and collected for
analysis, wherein
the puff of aerosol has a puff volume of 55 millilitres as generated by a
smoking machine.
Accordingly, any reference herein to a "puff" of aerosol should be understood
to refer to a 55
millilitre puff unless stated otherwise.
The ranges indicated define the total amount of each component measured in a
55 millilitre
puff of aerosol. The aerosol may be generated from an aerosol-generating
substrate using any
suitable means and may be trapped and analysed as described above in order to
identify the
characteristic compounds within the aerosol and measure the amounts thereof.
For example,
the "puff" may correspond to a 55 millilitre puff taken on a smoking machine
such as that used
in the Health Canada test method described herein.
Preferably, the aerosol according to the present invention comprises at least
about 0.1
microgram of ursolic acid per puff of aerosol, more preferably at least about
0.5 microgram of
ursolic acid per puff of aerosol. Alternatively, or in addition, the aerosol
generated from the
aerosol-generating substrate comprises up to about 5 micrograms of ursolic
acid per puff of
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aerosol, preferably up to about 4 micrograms of ursolic acid per puff of
aerosol and more
preferably up to about 3 micrograms of ursolic acid per puff of aerosol. For
example, the aerosol
generated from the aerosol-generating substrate may comprise between about
0.04 micrograms
and about 5 micrograms of ursolic acid per puff of aerosol, or between about
0.1 micrograms of
ursolic acid per puff of aerosol and about 4 micrograms of ursolic acid per
puff of aerosol, or
between about 0.5 microgram and about 3 micrograms of ursolic acid per puff of
aerosol.
Preferably, the aerosol according to the present invention comprises at least
about 0.05
microgram of isothymol per puff of aerosol, more preferably at least about 0.2
micrograms of
isothymol per puff of aerosol. Alternatively, or in addition, the aerosol
generated from the
aerosol-generating substrate preferably comprises up to about 1.25 micrograms
of isothymol
per puff of aerosol, more preferably up to about 1 microgram of isothymol per
puff of aerosol,
even more preferably up to about 0.75 micrograms of isothymol per puff of
aerosol. For
example, the aerosol generated from the aerosol-generating substrate may
comprise between
about 0.01 micrograms and about 1.25 micrograms of isothymol per puff of
aerosol, or between
about 0.05 microgram and about 1 microgram of isothymol per puff of aerosol,
or between about
0.2 micrograms and about 0.75 microgram of isothymol per puff of aerosol.
Preferably, the aerosol according to the present invention comprises at least
about 0.05
microgram of thymohydroquinone per puff of aerosol, more preferably at least
about 0.1
micrograms of thymohydroquinone per puff of aerosol. Alternatively, or in
addition, the aerosol
generated from the aerosol-generating substrate preferably comprises up to
about 1.25
micrograms of thymohydroquinone per puff of aerosol, more preferably up to
about 1
micrograms of thymohydroquinone per puff of aerosol, even more preferably up
to about 0.75
micrograms of thymohydroquinone per puff of aerosol. For example, the aerosol
generated
from the aerosol-generating substrate may comprise between about 0.01
micrograms and about
1.25 micrograms of thymohydroquinone per puff of aerosol, or between about
0.05 micrograms
and about 1 microgram of thymohydroquinone per puff of aerosol, or between
about 0.2
micrograms and about 0.75 micrograms of thymohydroquinone per puff of aerosol.
According to the present invention, the aerosol composition is such that the
amount of
ursolic acid per puff of aerosol is preferably at least 2 times the amount of
isothymol per puff of
aerosol. The ratio of ursolic acid to isothymol in the aerosol is therefore
preferably at least about
2:1. Preferably, the aerosol composition is such that the amount of ursolic
acid per puff of
aerosol is at least three times the amount of isothymol per puff of aerosol.
According to the present invention, the aerosol composition is such that the
amount of
ursolic acid per puff of aerosol is preferably at least 2 times the amount of
thymohydroquinone
per puff of aerosol. The ratio of ursolic acid to thymohydroquinone in the
aerosol is therefore
preferably at least about 2:1. Preferably, the aerosol composition is such
that the amount of
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ursolic acid per puff of aerosol is at least 3 times the amount of
thymohydroquinone per puff of
aerosol.
The defined ratios of ursolic acid to isothymol and thymohydroquinone
characterise an
aerosol that is derived from oregano particles. In contrast, in an aerosol
produced from oregano
essential oil, the ratios of isothymol to ursolic acid and thymohydroquinone
would be significantly
different.
Preferably, the aerosol according to the invention further comprises at least
about 0.1
milligrams of aerosol former per puff of aerosol, more preferably at least
about 0.2 milligrams of
aerosol per puff of aerosol and more preferably at least about 0.3 milligrams
of aerosol former
per puff of aerosol. Preferably, the aerosol comprises up to 0.6 milligrams of
aerosol former per
puff of aerosol, more preferably up to 0.5 milligrams aerosol former per puff
of aerosol, more
preferably up to 0.4 milligrams aerosol former per puff of aerosol. For
example, the aerosol may
comprise between about 0.1 milligrams and about 0.6 milligrams of aerosol
former per puff of
aerosol, or between about 0.2 milligrams and about 0.5 milligrams of aerosol
former per puff of
aerosol, or between about 0.3 milligrams and about 0.4 milligrams of aerosol
former per puff of
aerosol. These values are based on a puff volume of 55 millilitres, as defined
above.
Suitable aerosol formers for use in the present invention are set out above.
Preferably, the aerosol produced from an aerosol-generating substrate
according to the
present invention further comprise at least about 2 micrograms of nicotine per
puff of aerosol,
more preferably at least about 20 microgram of nicotine per puff of aerosol,
more preferably at
least about 40 micrograms of nicotine per puff of aerosol. Preferably, the
aerosol comprises up
to about 200 micrograms of nicotine per puff of aerosol, more preferably up to
about 150
micrograms of nicotine per puff of aerosol, more preferably up to about 75
micrograms of
nicotine per puff of aerosol. For example, the aerosol may comprise between
about 2
micrograms and about 200 micrograms of nicotine per puff of aerosol, or
between about 20
microgram and about 150 micrograms of nicotine per puff of aerosol, or between
about 40
micrograms and about 75 micrograms of nicotine per puff of aerosol. These
values are based
on a puff volume of 55 millilitres, as defined above. In some embodiments of
the present
invention, the aerosol may contain zero micrograms of nicotine.
Alternatively or in addition, the aerosol according to the present invention
may optionally
further comprise at least about 0.5 milligrams of a cannabinoid compound per
puff of aerosol,
more preferably at least about 1 milligram of a cannabinoid compound per puff
of aerosol, more
preferably at least about 2 milligrams of a cannabinoid compound per puff of
aerosol. Preferably,
the aerosol comprises up to about 5 milligrams of a cannabinoid compound per
puff of aerosol,
more preferably up to about 4 milligrams of a cannabinoid compound per puff of
aerosol, more
preferably up to about 3 milligrams of a cannabinoid compound per puff of
aerosol. For example,
the aerosol may comprise between about 0.5 milligrams and about 5 milligrams
of a cannabinoid
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compound per puff of aerosol, or between about 1 milligram and about 4
milligrams of a
cannabinoid compound per puff of aerosol, or between about 2 milligrams and
about 3
milligrams of a cannabinoid compound per puff of aerosol. In some embodiments
of the present
invention, the aerosol may contain zero micrograms of cannabinoid compound.
These values
are based on a puff volume of 55 millilitres, as defined above.
Preferably, the cannabinoid compound is selected from CBD and THC. More
preferably,
the cannabinoid compound is CBD.
Carbon monoxide may also be present in the aerosol according to the invention
and may
be measured and used to further characterise the aerosol. Oxides of nitrogen
such as nitric
oxide and nitrogen dioxide may also be present in the aerosol and may be
measured and used
to further characterise the aerosol.
The aerosol according to the invention comprising the characteristic compounds
from
the oregano particles may be formed of particles having a mass median
aerodynamic diameter
(MMAD) in the range of about 0.01 to 200 microns, or about 1 to 100 microns.
Preferably, where
the aerosol comprises nicotine as described above, the aerosol comprises
particles having a
MMAD in the range of about 0.1 to about 3 microns in order to optimise the
delivery of nicotine
from the aerosol.
The mass median aerodynamic diameter (MMAD) of an aerosol refers to the
aerodynamic diameter for which half the particulate mass of the aerosol is
contributed by
particles with an aerodynamic diameter larger than the MMAD and half by
particles with an
aerodynamic diameter smaller than the MMAD. The aerodynamic diameter is
defined as the
diameter of a spherical particle with a density of 1 gicnn3 that has the same
settling velocity as
the particle being characterised.
The mass median aerodynamic diameter of an aerosol according to the invention
may
be determined in accordance with Section 2.8 of Schaller et al., "Evaluation
of the Tobacco
Heating System 2.2. Part 2: Chemical composition, genotoxicity, cytotoxicity
and physical
properties of the aerosol," Regul. Toxicol. and Pharmacol., 81(2016) S27-S47.
As defined above, the invention further provides an aerosol-generating article
comprising
an aerosol-generating substrate, the aerosol-generating substrate comprising a
homogenised
oregano material, wherein upon heating of the aerosol-generating substrate
according to Test
Method A, the aerosol generated from the aerosol-generating substrate
comprises: ursolic acid
in an amount of at least 0.04 micrograms per puff of aerosol; isothymol in an
amount of at least
0.01 micrograms per puff of aerosol; and thymohydroquinone in an amount of at
least 0.01
micrograms per puff of aerosol, wherein a puff of aerosol has a volume of 55
millilitres as
generated by a smoking machine.
For the purposes of the present invention, a "puff" is defined as a volume of
aerosol
released from an aerosol-generating substrate upon heating and collected for
analysis, wherein
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the puff of aerosol has a puff volume of 55 millilitres as generated by a
smoking machine.
Accordingly, any reference herein to a "puff" of aerosol should be understood
to refer to a 55
millilitre puff unless stated otherwise. The ranges indicated define the total
amount of each
component measured in a 55 millilitre puff of aerosol. The aerosol may be
generated from an
aerosol-generating substrate using any suitable means and may be trapped and
analysed as
described above in order to identify the characteristic compounds within the
aerosol and
measure the amounts thereof. For example, the "puff" may correspond to a 55
millilitre puff
taken on a smoking machine such as that used in the Health Canada test method
described
herein.
Preferably, the amount of ursolic acid per puff of aerosol is at least 2 times
the amount
of isothymol per puff of aerosol, more preferably at least 3 times the amount
of isothymol per
puff of aerosol.
Preferably, the amount of ursolic acid per puff of aerosol is at least 2 times
the amount
of thymohydroquinone per puff of aerosol, more preferably at least 3 times the
amount of
thymohydroquinone per puff of aerosol.
As defined above, the present invention also provides an aerosol-generating
substrate
formed of a homogenised plant material comprising oregano particles, an
aerosol former and a
binder, wherein the aerosol-generating substrate comprises: at least 50
micrograms of ursolic
acid per gram of the substrate, on a dry weight basis; at least 5 micrograms
of isothymol per
gram of the substrate, on a dry weight basis; and at least 1.5 micrograms of
thymohydroquinone
per gram of the substrate, on a dry weight basis.
Below, there is provided a non-exhaustive list of non-limiting examples. Any
one or more
of the features of these examples may be combined with any one or more
features of another
example, embodiment, or aspect described herein.
EX1. An
aerosol-generating article comprising an aerosol-generating substrate, the
aerosol-generating substrate including a homogenised oregano material, the
homogenised
oregano material comprising oregano particles, an aerosol former and a binder,
wherein the
aerosol-generating substrate comprises:
at least 50 micrograms of ursolic acid per gram of the substrate, on a dry
weight basis;
at least 5 micrograms of isothymol per gram of the substrate, on a dry weight
basis; and
at least 1.5 micrograms of thymohydroquinone per gram of the substrate, on a
dry weight
basis.
EX2.
An aerosol-generating article according to example EX1 wherein the
amount of
ursolic acid per gram of the substrate is at least 8 times the amount of
isothymol per gram of the
substrate.
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EX3. An aerosol-generating article according to example EX1 or EX2 wherein
the
amount of ursolic acid per gram of the substrate is at least 25 times the
amount of
thymohydroquinone per gram of the substrate.
EX4. An aerosol-generating article according to example EX1, EX2 or EX3
wherein
the aerosol-generating substrate comprises between 50 micrograms and 6000
micrograms of
ursolic acid per gram of the substrate on a dry weight basis.
EX5. An aerosol-generating article according to any one of examples EX1 to
EX4
wherein the aerosol-generating substrate comprises between 5 micrograms and
600
micrograms of isothymol per gram of the substrate on a dry weight basis.
EX6. An
aerosol-generating article according to any one of examples EX1 to EX5
wherein the aerosol-generating substrate comprises between 1.5 micrograms and
200
micrograms of thymohydroquinone per gram of the substrate on a dry weight
basis.
EX7.
An aerosol-generating article according to any one of examples EX1 to
EX6,
wherein upon heating of the aerosol-generating substrate according to Test
Method A, an
aerosol is generated comprising:
at least 1.5 micrograms of ursolic acid per gram of the substrate, on a dry
weight basis;
at least 0.5 microgram of isothymol per gram of the substrate, on a dry weight
basis; and
at least 0.5 microgram of thymohydroquinone per gram of the substrate, on a
dry weight
basis.
EX8. An
aerosol-generating article according to example EX7, wherein upon heating
of the aerosol-generating substrate according to Test Method A, an aerosol is
generated
comprising up to 200 micrograms of ursolic acid per gram of the substrate, on
a dry weight basis.
EX9. An aerosol-generating article according to example EX7 or EX8, wherein
upon
heating of the aerosol-generating substrate according to Test Method A, an
aerosol is generated
comprising up to 50 micrograms of isothymol per gram of the substrate, on a
dry weight basis.
EX10. An aerosol-generating article according to example EX7, EX8 or EX9,
wherein
upon heating of the aerosol-generating substrate according to Test Method A,
an aerosol is
generated comprising up to 50 micrograms of thymohydroquinone per gram of the
substrate, on
a dry weight basis.
EX11. An aerosol-generating article according to any one of examples EX7 to
EX10,
wherein upon heating of the aerosol-generating substrate according to Test
Method A, an
aerosol is generated comprising zero micrograms of nicotine per gram of the
substrate.
EX12. An aerosol-generating article according to any one of examples EX1 to
EX6,
wherein upon heating of the aerosol-generating substrate in a THS2.2 holder
under the Health
Canada machine-smoking regimen, an aerosol is generated comprising:
at least 1.5 micrograms of ursolic acid per gram of the substrate, on a dry
weight basis;
at least 0.5 microgram of isothymol per gram of the substrate, on a dry weight
basis; and
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at least 0.5 microgram of thymohydroquinone per gram of the substrate, on a
dry weight
basis.
EX13. An aerosol-generating article according to any one of examples EX1 to
EX12,
wherein the homogenised oregano material comprises at least 0.5 percent by
weight of the
oregano particles, on a dry weight basis.
EX14. An aerosol-generating article according to any one of examples EX1 to
EX13,
wherein the homogenised oregano material comprises up to 50 percent by weight
of the oregano
particles, on a dry weight basis.
EX15. An aerosol-generating article according to any one of examples EX1 to EX
14,
wherein the homogenised oregano material further comprises up to about 75
percent by weight
of tobacco particles, on a dry weight basis.
EX16. An aerosol-generating article according to any one of examples EX1 to
EX15,
wherein the homogenised oregano material further comprises tobacco particles
and wherein the
weight ratio of oregano particles to tobacco particles is no more than 1:4.
EX17. An aerosol-generating article according to example EX15 or EX16, wherein
the
homogenised oregano material comprises between 5 percent and 20 percent by
weight of
oregano particles and between 55 percent and 70 percent by weight of tobacco
particles, on a
dry weight basis.
EX18. An aerosol generating article according to any one of examples EX1 to
EX17,
wherein the homogenised oregano material comprises substantially zero
nicotine.
EX19. An aerosol-generating article according to any one of examples EX1 to
EX17,
wherein the aerosol-generating substrate further comprises at least 0.1 mg of
nicotine per gram
of the substrate, on a dry weight basis.
EX20. An aerosol-generating article according to example EX19, wherein the
aerosol-
generating substrate comprises between 1 milligram and 20 milligrams of
nicotine per gram of
the substrate, on a dry weight basis.
EX21. An aerosol-generating article according to any one of examples EX1 to
EX20,
wherein the oregano particles have a D95 value of from greater than or equal
to about 50
microns to a D95 value of less than or equal to about 400 microns.
EX22. An aerosol-generating article according to any one of examples EX1 to
EX21,
wherein the oregano particles have a D5 value of from greater than or equal to
about 10 microns
to a D5 value of less than or equal to about 50 microns.
EX23. An aerosol-generating article according to any one of examples EX1 to
EX22,
wherein the oregano particles are purposely ground.
EX24. An aerosol-generating article according to any one of examples EX1 to
EX23,
wherein the diameter of 100 percent of the oregano particles is less than or
equal to 300 microns.
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EX25. An aerosol-generating article according to any one of examples EX1 to
EX24,
wherein the homogenised oregano material comprises up to 75 percent by weight
of particulate
plant material, the particulate plant material comprising the oregano
particles.
EX26. An aerosol-generating article according to any one of examples EX1 to
EX25,
wherein the homogenised oregano material has an aerosol former content of
between 5 percent
and about 30 percent by weight on a dry weight basis.
EX27. An aerosol-generating article according to any one of examples EX1 to
EX26,
wherein the binder is selected from: gums such as, for example, guar gum,
xanthan gum, arabic
gum and locust bean gum; cellulosic binders such as, for example,
hydroxypropyl cellulose,
carboxymethyl cellulose, hydroxyethyl cellulose, methyl cellulose and ethyl
cellulose;
polysaccharides such as, for example, starches, organic acids, such as alginic
acid, conjugate
base salts of organic acids, such as sodium-alginate, agar and pectins; and
combinations
thereof.
EX28. An aerosol-generating article according to any one of examples EX1 to
EX27,
wherein the binder comprises guar gum.
EX29. An aerosol-generating article according to any one of examples EX1 to
EX28,
wherein the homogenised oregano material comprises between 1 percent by weight
and 10
percent by weight of binder, on a dry weight basis.
EX30. An aerosol-generating article according to any one of examples EX1 to
EX29,
wherein the homogenised oregano material further comprises fibers.
EX31. An aerosol-generating article according to example EX30, wherein the
fibres
have lengths of greater than 400 micrometers.
EX32. An aerosol-generating article according to example EX30 or EX31, wherein
the
fibers are present in an amount of between about 2 percent by weight and about
15 percent by
weight, based on the dry weight of the aerosol-generating substrate.
EX33. An aerosol generating article according to example EX30 or EX31, wherein
the
fibers are present in an amount of at least 30 percent by weight, based on the
dry weight of the
aerosol-generating substrate.
EX34. An aerosol-generating article according to any one of examples EX1 to
EX33,
wherein the homogenised oregano material comprises oregano particles, between
about 5
percent by weight and about 30 percent by weight of aerosol former and between
about 1
percent by weight and about 10 percent by weight of binder, on a dry weight
basis.
EX35. An aerosol-generating article according to example EX34, wherein the
homogenised oregano material further comprises between about 2 percent by
weight and about
15 percent by weight of fibers.
EX36. An aerosol-generating article according to example EX34 or EX35, wherein
the
binder is guar gum.
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EX37. An aerosol-generating article according to any one of examples EX1 to
EX36,
wherein the homogenised oregano material is in the form of one or more sheets.
EX38. An aerosol-generating article according to example EX37, wherein each of
the
one or more sheets have a thickness of between 100 micrometres and 600
micrometres.
EX39. An aerosol-generating article according to example EX38, wherein each of
the
one or more sheets have a grammage of between 100 g/m2 and 300 g/m2.
EX40. An aerosol-generating article according to example EX38 or EX39, wherein
each
of the one or more sheets have a density of from 0.3 g/cm3to 1.3 g/cm3.
EX41. An aerosol-generating article according to example EX38, EX39 or EX40,
wherein each of the one or more sheets have a tensile strength at peak in a
cross direction of
from 50 N/m to 400 N/m.
EX42. An aerosol-generating article according to any one of examples EX38 to
EX40,
wherein each of the one or more sheets have a tensile strength at peak in a
machine direction
of from 100 N/m to 800 N/m.
EX43. An aerosol-generating article according to any one of examples EX38 to
EX42,
wherein the one or more sheets are in the form of one or more gathered sheets.
EX44. An aerosol-generating article according to any one of examples EX1 to
EX36,
wherein the homogenised oregano material is in the form of a plurality of
strands.
EX45. An aerosol-generating article according to example EX44, wherein the
width of
the strands is at least 0.2 mm.
EX46. An aerosol-generating article according to example EX44 or EX45, wherein
the
plurality of strands extend substantially longitudinally along the length of
the aerosol-generating
substrate, aligned with the longitudinal axis.
EX47. An aerosol-generating article according to example EX44, EX45 or EX46,
wherein the plurality of strands each have a mass to surface area ratio of at
least 0.02 milligrams
per square millimetre.
EX48. An aerosol-generating article according any one of examples EX1 to EX47,
wherein the homogenised oregano material in the aerosol-generating substrate
is in the form of
cast leaf.
EX49. An aerosol-generating article according any one of examples EX1 to EX47,
wherein the homogenised oregano material in the aerosol-generating substrate
is in the form of
oregano paper.
EX50. An aerosol-generating article according to any one of examples EX1 to
EX49,
wherein upon heating of the aerosol-generating substrate according to Test
Method A, the
aerosol generated from the aerosol-generating substrate comprises:
ursolic acid in an amount of at least 0.04 micrograms per puff of aerosol;
isothymol in an amount of at least 0.01 micrograms per puff of aerosol; and
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thymohydroquinone in an amount of at least 0.01 micrograms per puff of
aerosol,
wherein a puff of aerosol has a volume of 55 millilitres as generated by a
smoking
machine, wherein the amount of ursolic acid per puff of aerosol is at least 2
times the amount of
isothymol per puff of aerosol and wherein the amount of ursolic acid per puff
of aerosol is at
least 2 times the amount of thymohydroquinone per puff of aerosol.
EX51. An aerosol-generating article comprising an aerosol-generating
substrate, the
aerosol-generating substrate including a homogenised oregano material
comprising oregano
particles, between about 5 percent by weight and about 30 percent by weight of
aerosol former
and between about 1 percent by weight and about 10 percent by weight of
binder, on a dry
weight basis.
EX52. An aerosol-generating article according to example EX51, wherein the
homogenised oregano material further comprises an essential oil, preferably an
oregano
essential oil.
EX53. An aerosol-generating article according to examples EX51 or EX52,
wherein the
homogenised oregano material further comprises tobacco particles.
EX54. An aerosol-generating article according to any one of examples EX51 to
EX53,
wherein the homogenised oregano material comprises at least 0.5% by weight of
oregano
particles, on a dry weight basis.
EX55. An aerosol-generating substrate comprising a homogenised oregano
material
comprising oregano particles, aerosol former and binder, wherein the aerosol-
generating
substrate comprises:
at least 50 micrograms of ursolic acid per gram of the substrate, on a dry
weight basis;
at least 5 micrograms of isothymol per gram of the substrate, on a dry weight
basis; and
at least 1.5 micrograms of thymohydroquinone per gram of the substrate, on a
dry weight
basis.
EX56. An aerosol-generating system comprising:
an aerosol-generating device comprising a heating element; and
an aerosol-generating article according to any of examples EX1 to EX54.
EX57. An aerosol-generating system according to example EX56, wherein the
heating
element is a heater blade adapted to be inserted into the aerosol-generating
substrate.
EX57. An aerosol produced upon heating of an aerosol-generating substrate
according
to example EX55, the aerosol comprising:
ursolic acid in an amount of at least 0.04 micrograms per puff of aerosol;
isothymol in an amount of at least 0.01 micrograms per puff of aerosol; and
thymohydroquinone in an amount of at least 0.01 micrograms per puff of
aerosol,
wherein a puff of aerosol has a volume of 55 millilitres as generated by a
smoking
machine, wherein the amount of ursolic acid per puff of aerosol is at least 2
times the amount of
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isothymol per puff of aerosol and wherein the amount of ursolic acid per puff
of aerosol is at
least 2 times the amount of thymohydroquinone per puff of aerosol.
EX58. A method of making an aerosol-generating substrate comprising the steps
of:
forming a slurry comprising oregano particles, water, an aerosol former, a
binder and
optionally tobacco particles;
casting or extruding the slurry in the form of a sheet or strands; and
drying the sheet or strands at between 80 and 160 degrees Celsius.
EX59. A method according to example EX58, wherein the slurry is cast onto a
supportive surface and dried to form a sheet of cast leaf.
EX60. A method of making an aerosol-generating substrate comprising the steps
of:
forming a dilute suspension comprising oregano particles, water and optionally
tobacco
particles;
separating the suspension into an insoluble portion and a liquid extract;
forming the insoluble portion into a sheet;
concentrating the liquid extract and adding the concentrated liquid extract to
the sheet to
form an oregano paper.
Specific embodiments will be further described, by way of example only, with
reference
to the accompanying drawings in which:
Figure 1 illustrates a first embodiment of a substrate of an aerosol-
generating article as
described herein;
Figure 2 illustrates an aerosol-generating system comprising an aerosol-
generating
article and an aerosol-generating device comprising an electric heating
element;
Figure 3 illustrates an aerosol-generating system comprising an aerosol-
generating
article and an aerosol-generating device comprising a combustible heating
element;
Figures 4a and 4b illustrate a second embodiment of a substrate of an aerosol-
generating article as described herein;
Figure 5 illustrates a third embodiment of a substrate of an aerosol-
generating article as
described herein;
Figures 6a, 6b and 6c each show a cross sectional view of filter 1050 further
comprising
an aerosol-modifying element, wherein
Figure 6a illustrates the aerosol-modifying element in the form of a spherical
capsule or bead within a filter plug.
Figure 6b illustrates the aerosol-modifying element in the form of a thread
within
a filter plug.
Figure 6c illustrates the aerosol-modifying element in the form of a spherical
capsule within a cavity within the filter;
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Figure 7 is a cross sectional view of a plug of aerosol-generating substrate
1020 further
comprising an elongate susceptor element; and
Figure 8 illustrates an experimental set-up for collecting aerosol samples to
be analysed
in order to measure characteristic compounds.
Figure 1 illustrates a heated aerosol-generating article 1000 comprising a
substrate as
described herein. The article 1000 comprises four elements; the aerosol-
generating substrate
1020, a hollow cellulose acetate tube 1030, a spacer element 1040, and a
mouthpiece filter
1050. These four elements are arranged sequentially and in coaxial alignment
and are
assembled by a cigarette paper 1060 to form the aerosol-generating article
1000. The article
1000 has a mouth-end 1012, which a user inserts into his or her mouth during
use, and a distal
end 1013 located at the opposite end of the article to the mouth end 1012. The
embodiment of
an aerosol-generating article illustrated in Figure 1 is particularly suitable
for use with an
electrically-operated aerosol-generating device comprising a heater for
heating the aerosol-
generating substrate.
When assembled, the article 1000 is about 45 millimetres in length and has an
outer
diameter of about 7.2 millimetres and an inner diameter of about 6.9
millimetres.
The aerosol-generating substrate 1020 comprises a plug formed from a sheet of
homogenised oregano material comprising oregano particles, either alone or in
combination with
tobacco particles.
A number of examples of a suitable homogenised oregano material for forming
the
aerosol-generating substrate 1020 are shown in Table 1 below (see Samples B to
D). The sheet
is gathered, crimped and wrapped in a filter paper (not shown) to form the
plug. The sheet
includes additives, including glycerol as an aerosol former.
An aerosol-generating article 1000 as illustrated in Figure 1 is designed to
engage with
an aerosol-generating device in order to be consumed. Such an aerosol-
generating device
includes means for heating the aerosol-generating substrate 1020 to a
sufficient temperature to
form an aerosol. Typically, the aerosol-generating device may comprise a
heating element that
surrounds the aerosol-generating article 1000 adjacent to the aerosol-
generating substrate
1020, or a heating element that is inserted into the aerosol-generating
substrate 1020.
Once engaged with an aerosol-generating device, a user draws on the mouth-end
1012
of the smoking article 1000 and the aerosol-generating substrate 1020 is
heated to a
temperature of about 375 degrees Celsius. At this temperature, volatile
compounds are evolved
from the aerosol-generating substrate 1020. These compounds condense to form
an aerosol.
The aerosol is drawn through the filter 1050 and into the user's mouth.
Figure 2 illustrates a portion of an electrically-operated aerosol-generating
system 2000
that utilises a heating blade 2100 to heat an aerosol-generating substrate
1020 of an aerosol-
generating article 1000. The heating blade is mounted within an aerosol
article receiving
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chamber of an electrically-operated aerosol-generating device 2010. The
aerosol-generating
device defines a plurality of air holes 2050 for allowing air to flow to the
aerosol-generating article
1000. Air flow is indicated by arrows on Figure 2. The aerosol-generating
device comprises a
power supply and electronics, which are not illustrated in Figure 2. The
aerosol-generating
article 1000 of Figure 2 is as described in relation to Figure 1.
In an alternative configuration shown in Figure 3, the aerosol-generating
system is
shown with a combustible heating element. While the article 1000 of Figure 1
is intended to be
consumed in conjunction with an aerosol-generating device, the article 1001 of
Figure 3
comprises a combustible heat source 1080 that may be ignited and transfer heat
to the aerosol-
generating substrate 1020 to form an inhalable aerosol. The combustible heat
source 80 is a
charcoal element that is assembled in proximity to the aerosol-generating
substrate at a distal
end 13 of the rod 11. Elements that are essentially the same as elements in
Figure 1 have been
given the same numbering.
Figures 4a and 4b illustrate a second embodiment of a heated aerosol-
generating article
4000a, 4000b. The aerosol-generating substrate 4020a, 4020b comprises a first
downstream
plug 4021 formed from of particulate plant material comprising oregano
particles, and a second
upstream plug 4022 formed from particulate plant material comprising primarily
tobacco
particles. A suitable homogenised oregano material for use in the first
downstream plug is
shown in Table 1 below as one of Samples A to D. A suitable homogenised
tobacco material
for use in the second upstream plug is shown in Table 1 below as Sample E.
Sample E
comprises only tobacco particles and is included for the purposes of
comparison only.
In each of the plugs, the homogenised plant material is in the form of sheets,
which are
crimped and wrapped in a filter paper (not shown). The sheets both include
additives, including
glycerol as an aerosol former. In the embodiment shown in Figure 4a, the plugs
are combined
in an abutting end to end relationship to form the rod and are of equal length
of about 6 mm
each. In a more preferred embodiment (not shown), the second plug is
preferably longer than
the first plug, for example, preferably 2 mm longer, more preferably 3 mm
longer, such that the
second plug is 7 or 7.5 mm in length while the first plug is 5 or 4.5 mm in
length, to provide a
desired ratio of tobacco to oregano particles in the substrate. In Figure 4b,
the cellulose acetate
tube support element 1030 has been omitted.
The article 4000a, 4000b, analogously to the article 1000 in Figure 1, is
particularly
suitable for use with the electrically-operated aerosol-generating system 2000
comprising a
heater shown in Figure 2. Elements that are essentially the same elements in
Figure 1 have
been given the same numbering. It may be envisaged by the skilled person that
a combustible
heat source (not shown) may be instead be used with the second embodiment in
lieu of the
electrical heating element, in a configuration similar to the configuration
containing combustible
heat source 1080 in article 1001 of Figure 3.
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Figure 5 illustrates a third embodiment of a heated aerosol-generating article
5000. The
aerosol-generating substrate 5020 comprises a rod formed from a first sheet of
homogenised
oregano material formed of particulate plant material comprising a proportion
of oregano
particles, and a second sheet of homogenised tobacco material comprising
primarily cast-leaf
tobacco.
A suitable homogenised oregano material for use as the first sheet is shown in
Table 1
below as one of Samples A to D. A suitable homogenised tobacco material for
use as the
second sheet is shown in Table 1 below as Sample E. Sample E comprises only
tobacco
particles and is included for the purposes of comparison only.
The second sheet overlies the first sheet, and the combined sheets have been
crimped,
gathered and at least partially wrapped in a filter paper (not shown) to form
a plug that is part of
the rod. Both sheets include additives, including glycerol as an aerosol
former. The article 5000,
analogously to the article 1000 in Figure 1, is particularly suitable for use
with the electrically-
operated aerosol-generating system 2000 comprising a heater shown in Figure 2.
Elements
that are essentially the same elements in Figure 1 have been given the same
numbering. It
may be envisaged by the skilled person that a combustible heat source (not
shown) may be
instead be used with the third embodiment in lieu of the electrical heating
element, in a
configuration similar to the configuration containing combustible heat source
1080 in article 1001
of Figure 3.
Figures 6a, 6b and 6c are cross sectional views of filter 1050 further
comprising an
aerosol-modifying element. In Figure 6a, the filter 1050 further comprises an
aerosol-modifying
element in the form of a spherical capsule or bead 605.
In the embodiment of Figure 6a, the capsule or bead 605 is embedded in the
filter
segment 601 and is surrounded on all sides by the filter material 603. In this
embodiment, the
capsule comprises an outer shell and an inner core, and the inner core
contains a liquid
flavorant. The liquid flavorant is for flavouring aerosol during use of the
aerosol-generating article
provided with the filter. The capsule 605 releases at least a portion of the
liquid flavorant when
the filter is subjected to external force, for example by squeezing by a
consumer. In the
embodiment shown, the capsule is generally spherical, with a substantially
continuous outer
shell containing the liquid flavorant.
In the embodiment of Figure 6b, the filter segment 601 comprises a plug of
filter material
603 and a central flavour-bearing thread 607 that extends axially through the
plug of filter
material 603 parallel to the longitudinal axis of the filter 1050. The central
flavour-bearing thread
607 is of substantially the same length as the plug of filter material 603, so
that the ends of the
central flavour-bearing thread 607 are visible at the ends of the filter
segment 601. In Figure
6b, filter material 603 is cellulose acetate tow. The central flavour-bearing
thread 607 is formed
from twisted filter plug wrap and loaded with an aerosol-modifying agent.
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In the embodiment of Figure 6c, the filter segment 601 comprises more than one
plug of
filter material 603, 603'. Preferably, the plugs of filter material 603, 603'
are formed from
cellulose acetate, such that they are able to filter the aerosol provided by
the aerosol generating
article. A wrapper 609 is wrapped around and connects filter plugs 603, 603'.
Inside a cavity
611 is a capsule 605 comprising an outer shell and an inner core, and the
inner core contains a
liquid flavorant. The capsule is otherwise similar to the embodiment of Figure
6a.
Figure 7 is a cross sectional view of aerosol-generating substrate 1020
further
comprising an elongate susceptor strip 705. The aerosol-generating substrate
1020 comprises
a plug 703 formed from a sheet of homogenised oregano material comprising
tobacco particles
and oregano particles. The elongate susceptor strip 705 is embedded within the
plug 703 and
extends in a longitudinal direction between the upstream and downstream ends
of the plug 703.
During use, the elongate susceptor strip 705 heats the homogenised oregano
material by means
of induction heating, as described above.
Example
Different samples of homogenised plant material for use in an aerosol-
generating
substrate according to the invention, as described above with reference to the
figures, may be
prepared from aqueous slurries having compositions shown Table 1. Sample A
comprises only
oregano particles and no tobacco particles, in accordance with the invention.
Samples B to D
comprise oregano particles and tobacco particles, in accordance with the
invention. Sample E
comprises only tobacco particles and is included for the purposes of
comparison only.
The particulate plant material in all samples A to E accounts for
approximately 75 percent
of the dry weight of the homogenised plant material, with glycerol, guar gum
and cellulose fibers
accounting for the remaining approximately 25 percent of the dry weight of
homogenised plant
material. The samples are prepared from an aqueous slurry containing between
78-79kg of
water per 100kg of slurry.
In the table below, % DWB refers to the "dry weight base," in this case, the
percent by
weight calculated relative to the dry weight of the homogenised plant
material. The oregano
powder may be formed from dried oregano leaf, which may be ground to a final
D95 = 175
microns by triple impact milling.
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Table 1. Dry content of slurries
Cellulose
Oregano Tobacco Glycerol Guar Gum
Sample fibers
( /0 DWB) ( /0 DWB) ( /0 DWB) (% DWB)
(% DWB)
A 75 0 18 3 4
15 60 18 3 4
7.5 67.5 18 3 4
2.5 72.5 18 3 4
0 75 18 3 4
The slurries may be casted using a casting bar (0.6 mm) on a glass plate,
dried in an
oven at 140 degrees Celsius for 7 minutes, and then dried in a second oven at
120 degrees
Celsius for 30 seconds.
For each of the samples A to E of homogenised plant material, a plug may be
produced
from a single continuous sheet of the homogenised plant material, the sheets
each having
widths of between 100 mm to 125 mm. The individual sheets preferably have a
thickness of
about 235 microns and a grammage of about 180 g/m2. The cut width of each
sheet is about
132 mm. The sheets may be crimped to a height of 165 microns to 170 microns,
and rolled into
plugs having a length of about 12 mm and diameters of about 7 mm,
circumscribed by a paper
wrapper. The weight of homogenised plant material in each plug is about 285 mg
and the total
weight of each plug is about 293.6 mg.
For each of the plugs, an aerosol-generating article having an overall length
of about 45
mm may be formed having a structure as shown in Figure 3 comprising, from the
downstream
end: a mouth end cellulose acetate filter (about 7 mm long), an aerosol spacer
comprising a
crimped sheet of polylactic acid polymer (about 18 mm long), a hollow acetate
tube (about 8
mm long) and the plug of aerosol-generating substrate.
For Sample B of homogenised plant material, for which oregano particles make
up 20
percent of the particulate plant material, the characteristic compounds were
extracted from the
plug of homogenised plant material using methanol as detailed above. The
extract was
analysed as described above to confirm the presence of the characteristic
compounds and to
measure the amounts of the characteristic compounds. The results of this
analysis are shown
below in Table 2, wherein the amounts indicated correspond to the amount per
aerosol-
generating article, wherein the aerosol-generating substrate of the aerosol-
generating article
contained 285 mg of the Sample B of homogenised plant material.
For the purposes of comparison, the amounts of the characteristic compounds
present
in the particulate plant material (oregano particles) used to form Sample B
are also shown. For
the particulate material, the amounts indicated correspond to the amount of
the characteristic
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compound in a sample of particulate plant material having a weight
corresponding to the total
weight of the particulate plant material in the aerosol-generating article
containing 285 mg of
Sample B.
For each of the samples A, C and D comprising a proportion of oregano
particles, the
amount of the characteristic compounds can be estimated based on the values in
Table 2 by
assuming that the amount is present in proportion to the weight of the oregano
particles.
Table 2. Amount of oregano-specific compounds in the particulate plant
material
and in the aerosol-generating substrate
Characteristic Amount in the particulate Amount in the
aerosol-
Compound plant material generating substrate
(micrograms per article) (micrograms per
article)
Ursolic acid 440.5 466.3
I sothymol 389.2 40.2
Thymohydroquinone 5.1 12.9
Mainstream aerosols of the aerosol-generating articles incorporating aerosol-
generating
substrates formed from Samples A to E of homogenised plant material may be
generated in
accordance with Test Method A, as defined above. For each sample, the aerosol
that is
produced may be trapped and analysed.
As described in detail above, according to Test Method A, the aerosol-
generating articles
may be tested using the commercially available 1Q0S0 heat-not-burn device
tobacco heating
system 2.2 holder (THS2.2 holder) from Philip Morris Products SA. The aerosol-
generating
articles are heated under a Health Canada machine-smoking regimen over 30
puffs with a puff
volume of 55 ml, puff duration of 2 seconds and a puff interval of 30 seconds
(as described in
ISO/TR 19478-1:2014).
The aerosol generated during the smoking test is collected on a Cambridge
filter pad
and extracted with a liquid solvent. Figure 10 shows suitable apparatus for
generating and
collecting the aerosol from the aerosol-generating articles.
Aerosol-generating device 111 shown in Figure 10 is a commercially available
tobacco
heating device (1Q0S). The contents of the mainstream aerosol generated during
the Health
Canada smoking test as detailed above are collected in aerosol collection
chamber 113 on
aerosol collection line 120. Glass fiber filter pad 140 is a 44mm Cambridge
glass fiber filter pad
(CFP) in accordance with ISO 4387 and ISO 3308.
For LC-HRAM-MS analysis:
Extraction solvent 170, 170a, which in this case is methanol and internal
standard (ISTD)
solution, is present at a volume of 10 mL in each micro-impinger 160, 160a.
The cold baths
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161, 161a each contain a dry ice-isopropyl ether to maintain the micro-
impingers 160, 160a
each at approximately -60 C. The gas-vapour phase is trapped in the extraction
solvent 170,
170a as the aerosol bubbles through micro-impingers 160, 160a. The combined
solutions from
the two micro-impingers are isolated as impinger-trapped gas-vapor phase
solution 180 in step
181.
The CFP and the impinger-trapped gas-vapor phase solution 180 are combined in
a
clean Pyrex tube in step 190. In step 200, the total particulate matter is
extracted from the CFP
using the impinger-trapped gas-vapor phase solution 180 (which contains
methanol as a
solvent) by thoroughly shaking (disintegrating the CFP), vortexing for 5 min
and finally
centrifuging (4500 g, 5 min, 10 C). Aliquots (300 pL) of the reconstituted
whole aerosol extract
220 were transferred into a silanized chromatographic vial and diluted with
methanol (700 pL),
since the extraction solvent 170, 170a already comprised internal standard
(ISTD) solution. The
vials were closed and mixed for 5 minutes using an Eppendorf ThermoMixer (5
C; 2000 rpm).
Aliquots (1.5 pL) of the diluted extracts were injected and analyzed by LC-
HRAM-MS in
both full scan mode and data-dependent fragmentation mode for compound
identification.
For GCxGC-TOFMS analysis:
As discussed above, when samples for GCxGC-TOFMS experiments are prepared,
different
solvents are suitable for extracting and analysing polar compounds, non-polar
compounds and
volatile compounds separated from whole aerosol. The experimental set-up is
identical to that
described with respect to sample collection for LC-HRAM-MS, with the
exceptions indicated
below.
Nonpolar & Polar
Extraction solvent 171,171a, is present at a volume of 10 mL and is an 80:20
v/v mixture
of dichlormethane and methanol, also containing retention-index marker (RIM)
compounds and
stable isotopically labeled internal standards (ISTD). The cold baths 162,
162a each contain a
dry ice-isopropanol mixture to maintain the micro-impingers 160, 160a each at
approximately -
78 C. The gas-vapor phase is trapped in the extraction solvent 171, 171a as
the aerosol bubbles
through micro-impingers 160, 160a. The combined solutions from the two micro-
impingers are
isolated as impinger-trapped gas-vapor phase solution 210 in step 182.
Nonpolar
The CFP and the impinger-trapped gas-vapor phase solution 210 are combined in
a
clean Pyrex tube in step 190. In step 200, the total particulate matter is
extracted from the CFP
using the impinger-trapped gas-vapor phase solution 210 (which contains
dichloromethane and
methanol as a solvent) by thoroughly shaking (disintegrating the CFP),
vortexing for 5 min and
finally centrifuging (4500 g, 5 min, 10 C) to isolate the polar and non-polar
components of the
whole aerosol extract 230.
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In step 250, an 10 mL aliquot 240 of the whole aerosol extract 230 was taken.
In step
260, a 10 mL aliquot of water is added, and the entire sample is shaken and
centrifuged. The
non-polar fraction 270 was separated, dried with sodium sulfate and analysed
by GCxGC-
TOFMS in full scan mode.
Polar
ISTD and RIM compounds were added to polar fraction 280, which was then
directly
analysed by GCxGC-TOFMS in full scan mode.
Each smoking replicate (n = 3) comprises the accumulated trapped and
reconstituted
non-polar fraction 270 and polar fraction 280 for each sample
Volatile Components
Whole aerosol was trapped using two micro-impingers 160, 160a in series.
Extraction
solvent 172, 172a, which in this case is N,N-dimethylformamide (DMF)
containing retention-
index marker (RIM) compounds and stable isotopically labeled internal
standards (ISTD), is
present at a volume of 10 mL in each micro-impinger 160, 160a. The cold baths
161, 161a each
contain a dry ice-isopropyl ether to maintain the micro-impingers 160, 160a
each at
approximately -60 C. The gas-vapor phase is trapped in the extraction solvent
170, 170a as
the aerosol bubbles through micro-impingers 160, 160a. The combined solutions
from the two
micro-impingers are isolated as a volatile-containing phase 211 in step 183.
The volatile-
containing phase 211 is analysed separately from the other phases and injected
directly into
the GCxGC-TOFMS using cool-on-column injection without further preparation.
Table 3 below shows the levels of the characteristic compounds from the
oregano
particles in the aerosol generated from an aerosol-generating article
incorporating Sample B of
homogenised plant material, including oregano particles only. For the purposes
of comparison,
Table 3 also shows the levels of the characteristic compounds in the aerosol
generated from an
aerosol-generating article incorporating Sample E of homogenised plant
material, including
tobacco particles only (and therefore not in accordance with the invention).
Table 3. Content of characteristic compounds in aerosol
Compound Sample B Sample B Sample B
Sample E
(micrograms (micrograms (micrograms
(micrograms
per article) per gram) per 55 ml puff)
per article)
Ursolic acid 12.4 43.5 1.0
0.1
I sothymol 3.5 12.3 0.3
0
Thymohydroquinone 3.5 12.3 0.3
0.2
In the aerosol generated from Sample B, relatively high levels of the
characteristic
compounds were measured. The ratio of ursolic acid to isothymol was above 1
and the ratio of
isothymol to thymohydroquinone was also above 8. The levels of the
characteristic compounds
were therefore indicative of the presence of oregano particles in the sample.
In contrast, for the
CA 03224451 2023- 12- 28

WO 2023/285597
PCT/EP2022/069746
-67-
tobacco only Sample E, which contained substantially no oregano particles, the
levels of the
characteristic compounds were found to be at or close to zero.
For each of the samples A, C and D comprising oregano particles, the amount of
the
characteristic compounds in the aerosol can be estimated based on the values
in Table 3 by
assuming that the amount is present in proportion to the weight of the oregano
particles in the
aerosol-generating substrate from which the aerosol is generated.
Table 4 below compares the levels of certain aerosol constituents in the
aerosol
generated from an aerosol-generating article incorporating sample B (20:80
ratio of oregano to
tobacco) with the aerosol generated from the tobacco only Sample E. The
reduction indicated
is the percentage reduction provided by replacing 20 percent of the tobacco
particles in the
homogenised material of Sample E with oregano particles.
As shown in Table 4, the aerosol produced from Sample B containing 20 percent
by
weight oregano particles based on the dry weight of the particulate plant
material results in
reduced levels of phenol, o-cresol and m-cresol when compared to the levels of
the same
compounds in the aerosol produced from Sample E containing 100 percent by
weight tobacco
based on the dry weight of the particulate plant material.
In most cases, the reduction provided in the level of these undesirable
aerosol
compounds is significantly greater than the proportional reduction that would
be expected as a
result of the substitution of 20 percent of tobacco particles for oregano
particles. The inclusion
of the oregano particles in combination with the tobacco particles is
therefore providing an
unexpectedly high reduction in the levels of these compounds. The inclusion of
oregano
particles can therefore provide an aerosol that has improved sensory
attributes whilst reducing
the levels of certain undesirable compounds in the aerosol.
Table 4. Composition of aerosol
Aerosol Constituent Sample E Sample B Reduction
(100% (20% oregano) (c)/0)
tobacco)
Phenol 1.501 0.926 38.6
(pg/article)
o-cresol 0.071 0.043 39.5
(pg/article)
m-cresol 0.033 0.021 34.6
(pg/article)
CA 03224451 2023- 12- 28

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États administratifs

2024-08-01 : Dans le cadre de la transition vers les Brevets de nouvelle génération (BNG), la base de données sur les brevets canadiens (BDBC) contient désormais un Historique d'événement plus détaillé, qui reproduit le Journal des événements de notre nouvelle solution interne.

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Pour une meilleure compréhension de l'état de la demande ou brevet qui figure sur cette page, la rubrique Mise en garde , et les descriptions de Brevet , Historique d'événement , Taxes périodiques et Historique des paiements devraient être consultées.

Historique d'événement

Description Date
Inactive : Page couverture publiée 2024-01-31
Exigences quant à la conformité - jugées remplies 2024-01-09
Exigences pour l'entrée dans la phase nationale - jugée conforme 2023-12-28
Demande de priorité reçue 2023-12-28
Exigences applicables à la revendication de priorité - jugée conforme 2023-12-28
Lettre envoyée 2023-12-28
Inactive : CIB en 1re position 2023-12-28
Inactive : CIB attribuée 2023-12-28
Inactive : CIB attribuée 2023-12-28
Inactive : CIB attribuée 2023-12-28
Inactive : CIB attribuée 2023-12-28
Inactive : CIB attribuée 2023-12-28
Demande reçue - PCT 2023-12-28
Demande publiée (accessible au public) 2023-01-19

Historique d'abandonnement

Il n'y a pas d'historique d'abandonnement

Taxes périodiques

Le dernier paiement a été reçu le 2024-07-01

Avis : Si le paiement en totalité n'a pas été reçu au plus tard à la date indiquée, une taxe supplémentaire peut être imposée, soit une des taxes suivantes :

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  • taxe additionnelle pour le renversement d'une péremption réputée.

Les taxes sur les brevets sont ajustées au 1er janvier de chaque année. Les montants ci-dessus sont les montants actuels s'ils sont reçus au plus tard le 31 décembre de l'année en cours.
Veuillez vous référer à la page web des taxes sur les brevets de l'OPIC pour voir tous les montants actuels des taxes.

Historique des taxes

Type de taxes Anniversaire Échéance Date payée
Taxe nationale de base - générale 2023-12-28
TM (demande, 2e anniv.) - générale 02 2024-07-15 2024-07-01
Titulaires au dossier

Les titulaires actuels et antérieures au dossier sont affichés en ordre alphabétique.

Titulaires actuels au dossier
PHILIP MORRIS PRODUCTS S.A.
Titulaires antérieures au dossier
DANIEL ARNDT
PRISCA CAMPANONI
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Description du
Document 
Date
(yyyy-mm-dd) 
Nombre de pages   Taille de l'image (Ko) 
Page couverture 2024-01-30 1 61
Dessin représentatif 2024-01-30 1 6
Description 2023-12-27 67 4 208
Revendications 2023-12-27 3 111
Dessins 2023-12-27 7 349
Abrégé 2023-12-27 1 14
Paiement de taxe périodique 2024-06-30 28 1 121
Demande d'entrée en phase nationale 2023-12-27 4 168
Traité de coopération en matière de brevets (PCT) 2023-12-27 1 73
Rapport de recherche internationale 2023-12-27 4 111
Demande d'entrée en phase nationale 2023-12-27 8 184
Traité de coopération en matière de brevets (PCT) 2023-12-27 1 63
Courtoisie - Lettre confirmant l'entrée en phase nationale en vertu du PCT 2023-12-27 2 49