Note: Descriptions are shown in the official language in which they were submitted.
CA 02099493 2002-05-03
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1
1PATER-SOLUBLE DELIVERY SY8TEM8 FOR BYl~ROPHOBIC. LIQQID8
BACKGROUND OF THE INPEIfrION
The present invention is directed t:o a novel method
of encapsulating finely divided or micranized,
substantially hydrophobic fluids using flash-flow, a:g.
melt-spun techniques, to produce delivex-y systems for use
in food products and other comestibles, pharmaceuticals,
gum and confectionery products, cosmetics and personal
hygiene products: More particularly, thae present
invention relates to a delivery system having a solid,
hydrophilic encapsulating material capable of undergoing
those changes associated with the flash-flow phenomena
occurring during, for example, melt spinning and having a
multitude of finely divided or micronized hydrophobic oil
dispersed therein.
The use of hydrophobic ails as flavorants or
fragrances in comestibles, pharmaceuticals, cosmetic's and
the like has focused on ways to control the organoleptic
impact either by delaying or accelerating the intensity of
perception. In conventional comestible products such as
foods, pharmaceuticals, gum and confectioneries, flavor
oils have been added in the free state, as well as in the
encapsulated form for the combined effects of immediate
and delayed flavor perception. For example, U.S. Patent
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Na. 4,485,118 to Carrol, et al: discloses a chewing gum
composition,which contains sequentially released plural
flavor system. One of the flavors is encapsulated with a _
water-insolublecoating for delayed release and a separate
flavor is introduced in free, uncoated form for immediate ..
release.
In the comestible art, encapsulation and coating
techniques have also focused on protecting the flavor oils
from reacting with other co-mixed chemicals, or from
oxidation, evaporation: orvolatilization through direct
exposure to the environment. Flavor oils have been
combined with a variety of sweeteners, particularly, for
example, in gum and confectionery products. Flavor oils
are often aldehyde, ketone and ester compounds.which ate
highly reaotive with a host of other common materials
found in comestible products, as well as being sensitive
to heat. For example, one such material commonly added to
comestibles which reacts quickly to lose its sweetness in
the presence of flavor oils is asparta~ae. The result is a
comestible product which lacks both flavor and sweetness
and therefore suffers front lack of overall organoleptic
quality and shelf-life instability.
Methods of encapsulat ng or coating oils have
conventionally involved using matrices of other
hydrophobic materials, such as melted and solidified fats
and waxes, polymers such as polyvinyl acetate and . '
solvents, and/or ela tomeric materials. Simple mi~c~tures -
of these hydrophobic matrices and the flavor and/or
sweetener materials were prepared using solvents and/or
heat to form a melt in order to incarporate the flavor oil
WO 93/08699 a., ; ~a ~ ~ ~ ~. ~~ ~ ~ ~ ~ i'~/Uf'92/094d7
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into the matrix. Incorporation in the melted stage was ,
required to obtain as much homogeneity and encapsulation
as possible. The molten mass was then cooled to
solidification and ground into particles.
U.S. Patent No. 4,?40,376 to Yang discloses use of a
melted high molecular weight polyvinylacetate blended with
a hydrophobic plasticizer and a flavoring ingredient. The
melt blend is cooled, ground into a particulate and
incorporated into an edible product. The hydrophobic
plasticizers employed are mono-, di- and triglycerides
having a fatty acid chain length of 16 to 22 carbons.
U.S. Patent No. 4,722,845 to Cherukuri, et al.
discloses stable cinnamon flavored chewing gum
compositions comprising gum base, sweetener and a
sweetener delivery system comprising a dipeptide or amino
acid sweetener in a mixture of fat and high melting point
(106°C) polyethylene wax. U.S. Patent No. 4,803,02 also
to Cherukuri, et al. discloses a powdered flavor y
composition encapsulated in a hydrophobic matrix of fat or
wax and containing thaumatin, monellin or dihydrochalcones
as the sweetener.
U.S. Fatent No. 4,824,681 to Schobel, et al.
discloses an encapsulated sweetening agent which is
protected from moisture and provides controlled release
wherein the sweetening agent is encapsulated with a
hydrophobic polymer and a hydrophobic plasticizer.
Hydrophobic coating is also described in detail in U.S.
Patent Na. 4,828,857 to Sharma, et a1. wherein a delivery
system is disclosed having as a 'core material a sweetener
or flavoring ingredient and a protective matrix formed by
a fluidized bed spray coating.
PCIC/U~92/U9447
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These processes involving the formation of molten
hydrophobic mixtures have inherent disadvantages which
include loss of volatile flavor components during the
heating process and significant mixing requiremewts to '
ensure homogeneity. Separate grinding steps followed,
which also generated vaporization of flavor components
and, in the case of certain sensitive sweeteners,
degradation and loss of sweetness. Additionally, simple
mixtures have failed to provide adequate uniform coating
protection to keep the core flavors arid sweeteners in a
sustained stabilized state. Other processes, in an
attempt to improve over simple mixing techniques, have
included spray congealing and fluidized bed spray coating.
While these methods may overcome certain of the above-
mentioned disadvantages, they still employ significant
amounts of heat and/or solvents and plasticizers and do
not result in micronized discrete flavor droplets within a
matrix, but rather a non-uniform agglomeration of 'the
flavor and/or sweetener with the hydrophobic carrier.
See, for example, U.S. Patent No. 4,722,x45 to Cherukuri,
et al. Coating of sweeteners and oils with hydrophobic
materials also interferes with the immediate release
properties and up-front, instantaneous flavor and/or
sweetness impact.
The delivery systems of the present invention
represents a departure from conventional methods and their
resultant products in a number of important ways. To
begin with, instead of using hydrophobic encapsulating
matrix materials, flash-flowable hydrophilic materials are
employed. These materials must be capable of undergoing
flash-flow processes such as melt-spinning without ,
significant degradation or burning. Therefore, instead of
simple mixing and grinding, spray congealing and spray ,
coating techniques, flash-flow processing as later defined
herein, is employed. The result is a solid particulate
which constitutes a highly water-soluble, flash-flowable
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matrix or encapsulant in which there is dispersed
throughout fine, micronized liquid droplets. During the
flash-flow process, the encapsulant is exposed to
extremely limited conditions of heat and then usually only
for a fraction of a second. This substantially lessens
the potential for volatilization of certain hydrophobic
liquid components. Tn the case of flavor oils, analytical
testing has demonstrated that the intensive delivery
systems retain more flavor components than those processes
of the prior art.
~U~~RSC OF 'f~E ~~d~Eld'fTOPI
The present invention concerns a method of producing
encapsulated hydrophobic fluids, and the resultant
delivery systems made therefrom. The oils are contained
in and protected by encapsulation in a water-soluble,
solid matrix made from flash-flowable materials such as
sweetening agents and the like. The oil is present in 'the
matrix in finely divided micronized droplets which are
dispersed in and entrapped by the surrounding matrix. The
encapsulated liquid particles result from the flash-flow
process, e.g., by melt-spinning a mixture of a water-
soluble matrix with the oil to produce flakes or floss
particles which can be used "as is" or subsequently
further divided into a fine powder. The powder is formed
of particles which in turn constitutes a matrix of 'the
water-soluble protective coating and a micronized oil
dispersion contained therein.
The preferred matrix materials are sweetening agents
which are readily processed through flash-flow processing
techniques. In one preferred embodiment the delivery
system employs flavor oils which are intended to be used
in comestible products. The combination of a sweet " ..
tasting water-soluble matrix and flavor or aromatic oil
dispersed throughout provides a synergistic effect due to
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the concurrent release of both constituents. It is
believed that the immediate delivery of the oil in the
mouth provides a fla~or/sweetener impact which is not only
more intense but more true to the original flavor oil
taste. This effect is due to the fact that more flavor
components'have been retained during processing and give a
higher perception of intensity due to their intimate
contact with the flash-flowable sweetener.
The flavor oils may be chosen from a host of
materials which are suitable for the chosen application.
Peppermint oil, for example, is one such oil which is
commonly used in chewing gum and confectionery products
and which when incorporated into the present delivery
system provides a means of protecting the o~.l from loss of
volatiles and degradation, yet produces immediate, up-
front flavor release when placed in the mouth or other
aqueous medium.
In one aspect of the invention, a particulate.
delivery system'having a hydrophobic liquid dispersion or
'core and a solid water-soluble matrix is produced by means
of flash-flow processing. The delivery system can be used
in a variety of, products for delivering hydrophobic oils,
and in particular, flavor, fragrance and other aromatic
oils. The delivery systemyis especially useful for
instant and immediate delivery of the core material upon
contact with mo~ature, e.g:, when placed in the mouth.
One particular application involves the use of the
delivery system as dusting powders for chewing gum,'
confectionery products and baked goods.
The delivery system of the present invention provides
uniform distribution of the hydrophobic liquid composition
and retains the volatile and unstable components of the
liquids which contribute to the overall character of the
liquid. In the case of flavor oils and various aromatic
pGT/LJ~921094.47
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oils, essential volatile components such as flavor notes
and aromas are retained during processing and captured in
the final product, which results in a more flavorful or
fragrant product with high authenticity and trueness to
its intended taste and/or smell.
The flash-flow process is essentially instantaneous
and vaporization and/or degradation of the hydrophobic
liquid composition, including other components such as
sweeteners or fibers carried therewith, is substantially,
l0 if not completely reduced when compared to conventional
spray-drying processing and simple mixincJ.
The delivery system can be used in applications such
as flavor and sweetener dusting powders without the use of
anti-caking materials such as corn starch. The delivery
~5 system emerges from the flash-flow process in a number of
different forms, such as floss or flakes, but can be
ground, pulverized or sieved into a fine particulate or
powder without substantial loss of hydrophabic liquid or
other components contained in the matrix. Cryogrinding
20 using nitrogen is the preferred method of cominution. The
retention of oil components in the inventive process is
largely due to the fact that the liquid is in micronized
form within the matrix rather than being simply adsorbed
onto a carrier or enrobed within a coating.
25 The delivery systems also have a more uniform
distribution of the hydrophabic liquid composition than .,,.
can be achieved by simple mixing or spray drying
techniques. One particular advantage is that a variety of
flash-flowable materials can be used in conjunction with
30 the hydrophobic oil to satisfy a host of applications.
For example, spray-dried mixtures of cyclodextrins and
flavors can be combined with the flash-flowable matriac
materials to provide enhanced flavor-delivexy systems.
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The flash-flow-formed delivery system retains substantially
all of its flavor components and can be cryoground to a
uniform particle size distribution. Cryogrinding has the
unique advantage over conventional grinding of reducing heat
build-up and subsequent loss of volatiles. This allows for
a greater uniformity in particle size and shape than
ordinary grinding, where frictional heat build-up can be
problematic. Very fine powders can be produced using flash-
flow processing followed by cryogrinding. These powders can
be directly applied to comestibles and have particular
application as flavor/sweetener delivery systems useful in
chewing gum compositions or dusting powders on gum and
confectionery surfaces. These powders readily adhere to
chewing gum surfaces during rolling and scoring of the gum
due to the uniform particle size and shape.
An embodiment of the above-mentioned method of the
present invention comprises, subjecting a flash-flowable
material to flash-flow conditions to form a solid
particulate comprising a matrix of the flash-flowable
material containing a micronized dispersion of the
hydrophobic liquid, wherein the flash-flowable matrix
incorporates a flash-flowable non-saccharide based polymer.
Another aspect of the present invention provides a
chewing gum. In one embodiment, the chewing gum comprises:
a) a gum base; and
b) a solid sweetener and flavor delivery system comprising a
water-soluble flash-flow-form matrix containing a micronized
dispersion of flavor oil.
In another embodiment, the chewing gum has a core
portion comprising a gum base, a sweetener and a flavor and
has deposited on a surface of the core portion a powdered
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rolling material comprising particles of flash-flow-formed
saccharide-based material containing a micronized dispersion
of a flavor oil.
A further aspect of the present invention provides
a comestible product having enhanced flavor comprising an
edible flash-flow-formed delivery system having a micronized
dispersion of a flavor oil contained in a water-soluble
flash-flowable material.
For a better understanding of the present
invention, references made to the following description and
its scope will be pointed out in the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
Figure 1 is a photomicrograph (500x) showing
micronized peppermint oil in a flash-flow-formed matrix of
Maltrin-365.
Figure 2 is a photomicrograph (500x) showing
micronized peppermint oil in a flash-flow-formed particulate
matrix of Maltrin-365 which has undergone cryogrinding.
Figure 3 is a photomicrograph (1250x) showing
micronized peppermint oil in flash-flow-formed matrix of an
isomalt.
~3'~ 93/08699 ; PCr/US92109447
f,~:°~:.:a
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Figure 4 is a photomicrograph (1250x) showing
micronized peppermint oil in a flash-flow-formed
particulate matrix of an isomalt which has undergone
cryogrinding.
Figure 5 is a graph showing a comparison of
volatilization retention of the flash-flow formed delivery
system, with and without cryogrinding, asc compared to
simple mixture encapsulation under contre>lled temperature
conditions.
DETAILED DESCRIPTIOTH OF THE ~~1~7ENTION
The present invention concerns the formation of a new
solid delivery system for rapid release of hydrophobic
liquids. The delivery system includes a matrix of water-
soluble flash-flowable material having a micronized
dispersion of hydrophobic liquid contained 'therein. The
matrix is designed to be protective of the oil during
processing, with little or no substantial loss of oil
components during the delivery system formation, yet be
readily releasable of the oil components in conditions of
moisture. In particular, the oils are immediately y
released in aqueous medium and especially when placed in
contact with the oral cavity or other moist conditions in
or on the body where rapid release of oil is desirable.
The hydrophobic liquid can be chosen from a variety
of materials such as oleaginous liquids, flavor or
aromatic oils as well as mineral oil, glycerin,
palyethylene glycol, and the like. Examples of oleaginous
liquids include, without limitation, vegetable oils, fish
oils, lard, lanolin, cocoa bwtter and mixtures thereof.
Tt will be appreciated that those hydrophobic materials
which are solid at room 'temperature can be used provided
they are rendered sufficiently liquid to be dispersed
within the matrix during processing. Alternatively, in
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209949 ~~-
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cases where the oleaginous material can be rendered to a
dispersible state with pre-heating withowt destroying or
losing desired volatile components, such limited pre- ,
heating may be employed. For example, animal fats such as
tallow, lard or hydrogenated animal and/or vegetable oils ,
can be employed in the present invention.
Hydrogenation or partially hydrogenated vegetable
oils useful in the present delivery systems include such
materials as corn oil, canola oil, cottonseed oil, sesame
oil, soybean oil, grape-seed oil, sunflower oil, safflower
oil, rapeseed oil, olive oil, peanut oil and the like.
These oils, as well as the animal fat oils are ingestible
and are therefore most commonly used in comestibles.
Other hydrophobic oils include those referred to as
flavor oils or essences. These oils are generally derived .
from plant extracts, although may alternatively be
synthetically derived. Peppermint oil, spearmint oil,
cinnamon oil, oil of wintergreen, citrus oils arid other
fruit essences are the most commonly used flavor oils
which are employed in the present invention. Flavor oils
such as peppermint oil, spearmint oil and cinnamon oil are
particularly harsh and create a burning sensation in the
mouth if ingested in too high a quantity. The present
invention allaws for the use of smaller quantities than in
typically comestible applications if desired due to the
synergy which is achieved with the sweetner matrix. The
micronized dispersion gives the perception that a greater
quantity of flavor is present than the actual amount,
thereby enhancing both the organoleptic impact with less
flavor oil and eliminating the need for higher amounts.
This is particularly useful in applications such as
chewing gum compositions, where the addition of flavor oil
at high concentrations to achieve a more intense flavor
impact results in plasticization of the gum base
components and sloppy chew characteristics.
I
W~ 93/0699 PCTlZJS92/09447
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Examples of citrus or first oils and/or essences
which are useful include a host of materials such as
apple, apricot, banana, blueberry, cherry, grape,
grapefruit, lemon, lime, orange, pear, peaches, pineapple,
plum, raspberry, strawberry and the like. Mixtures and
derivatives of these oils are contemplated.
Additional flavoring agents may be chosen from
synthetic flavor oils and flavoring aromatics, and/or
oils, oleo resins and extracts derived from plants,
leaves, flowers, fruits and so forth, arid combination
thereof. For example, clove oil, bay oil, anise oil, .
eucalyptus oil, thyme oil, cedar leaf oil, oil of nutmeg,
oil of sage, oil of bitter almonds and cassia oil may be
used. Commonly used flavors include menthol, artificial
vanilla, cinnamon derivatives, and various fruit flavors,
whether employed individually or in admixture.
Flavorings such as aldehydes and esters including
cinnamyl acetate, cinnamaldehyde, citral diethylacetal,
dihydrocarvyl acetate, eugenyl formate, p-methylamisol,
and so forth may also be used. Generally any flavoring or
food additive such as those described in °'Chemicals Used
in Food Processing,'° pub 1274 by the National Academy of
Sciences, pages 63-258 may be used.
Further examples of aldehyde flavorings include, but
era not limited to.acetaldehyde (apple): benzaldehyde
(cherry, almond), anisic aldehyde (licorice, anise)a
cinnamic aldehyde (cinnamon)a citral, i.e., alpha citral
(lemon, lime): neral, i.e. beta citral (lemon, lime);
decanal (orange, lemon); ethyl vanillin (vanilla, cream);
hellotropine, i.e., piperonal (vanilla, cream): vanillin
(vanilla, cream); alpha-amyl cinnamaldehyde (spicy fruity
flavors): butyraldehyde (butter, cheese); valcraldehyde
(butter, cheese): citronellal; decanal (citrus fruits);
aldehyde C-8 (citrus fruits); aldehyde C-9 (citrus .
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fruits); aldehyde C-12(citrus fruits),~ 2-
ethylbutyraldehyde (berry fruits); hexenal, i.e., traps-2
(bent' fruits): tolyl aldehyde (cherry, almond), -
veratraldehyde (vanilla); 2,6-dimethyl-5-heptenal, i:e.
Melonal (melon); 2,6-dimethyl-5-heptenal, i:e., Meianal -
(melon) ; 2, 6-dimethyloctanal (green fruit) ; and 2-
dodecenal (citrus, mandarin); cherry: gripe, strawb_erxy
shortcake; mixtures thereof; and the like.
other specific flavor compounds such as ethylacetate,
thiophene, ethylpropionate, ethyl butyrate, 2-hexanoate,
2-methylpyazine, heptaldehyde, 2-octanone, limonene, and
eugenol are also useful.
The hydrophobic oil content of the present delivery
systems is generally in the range of about 0.02% to about
40% by: weight of he delivery ystem. However, deviations
from this range ire certainly possible provided that the
micronized dispersion of the oil in the matrix results as
a result of the flash-flow process. Preferably, the oils
are present in amounts of about 0.5% to about 20% by'
weight of tyke delivery system and most preferably about 2%
to about 12%.
The matrix materials can be selected from any
m terial which is: capable: of undergoing those physical
and/or chemical changes associated with flash-flow
processing. Flash-flaw processing has been described in a
number of co~amonly owned patents such as U:S: Patent
4,855,326, 5,001,532 and 5,096,492 from which the present
application relates back, as well as 5,011,522 and w '.
4,873,085.
i
WO 93/08699 4 PCT/US92IQ9447
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Those materials useful as matrices may be chosen from
such classes as sugars or sugar derivatives. These types
of materials are preferred because of their flash-flow
capabilities and their wide variety of applications. The
term sugar is meant to include those carbohydrates having ,
a high glucose profile. A high glucose profile means that
the carbohydrate has a large number of six-carbon mono and
disaccharides as well as other glucose-based oligomers.
Mono-, di-, tri- and polysaccharides and their derivatives ;
may be employed. Examples include glucose, sucrose,
maltose, lactose, arabinose, xylose, ribose, fructose,
mannose, pentose, galactose, sorbose, dextrose, sorbitol,
xylitol, mannitol, pentatol, maltitol, isomalt, sucralose,
maltodextrin, polydextrose and mixtures thereof.
Other matrix materials include cellulosics and
starches and their chemical and biological derivatives.
Cellulosics, however, are generally added in combination
with mono- and disaccharide-based materials because the
cellulosics are not as easily processed alone using flash-
flow techniques.
The delivery systems of the present invention have a
substantially amorphous flash-flow-formed matrix. The
terms "flash-flow°' refers to a process of subjecting the
feedstock, e.g. matrix material and hydrophobic oil,
simultaneously to flash heating and applied physical force
such that the solid matrix material experiences sufficient
internal flow to transform it to a physically and/or
chemically altered structure from that of the feedstock.
Flash-flow processing can be accomplished several
ways. Flash heat and flash shear are two such processes
which can be used: In the flash heat process, the
feedstock material is heated sufficiently to create an
internal flow condition which permits part of the
feedstock to move at a subparticle level with respect to
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the rest of the mass and exit openings provided in the
i
perimeter of the spinning head. The centrifugal force
created in the spinning head flings the flowing feedstock
material outwardly from the head so that it reforms with a
changed structure. The force required to separate and , ;
discharge flowable feedstock is only centrifugal force
which results from the spinning head. The flash heat
process is one process far producing an amorphous matrix
such as the sugar floss used in this invention.
20 In the flash shear process, a shearform matrix is
formed by raising the temperature of the feedstock
material which includes a non-solubilized carrier to a
point where the carrier such as a saccharide-based
material undergoes internal flow upon application of a
fluid shear force. The feedstock is advanced and ejected
while in internal flow condition, and subjected to
disruptive fluid shear forces to form multiple parts or
masses which have morphology different from that of the
original feedstock.
The multiple masses are cooled substantially
immediately after contact with the fluid shear force and
are permitted to continue in a free-flow condition until
solidified.
The feedstock material which can be used in a flash
shear process includes but is not limited to a carrier
such as a saccharide-based material. Other materials such
as oleaginous materials can also be included in the
feedstock.
It is important that the feedstock selected for a
flash shear process have the ability to be processed .
without reliance upon dissolution. In the case of a
saccharide based material, the feedstock is prianarily a
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solid material which is subjected to the flash shear
process.
The flash shear process can be carried out in an
apparatus which has means for increasing the temperature
of a non-solubilized feetistock and means for
simultaneously advancing it for ejection. A multiple
heating zone twin screw extruder can be used for _
increasing the temperature and advancing feedstcckThe
second element of the apparatus is a'means for ejecting
the feedstock iri a condition' for shear~.ng it to provide
the shearform matrix. The means for ejecting is in fluid
communication with the means for increasing the
temperature and is arranged at the point to receive the
feedstock while it is in the internal flow conditions.
The means for ejecting the feedstock is preferably a
nozzle which provides high pressure ejection of the
feedstock material:
A preferred flash-flow process used to form the
inventive delivery systemswinvolves spinning a feedstock
in a "cotton candy" fabricating type machine. The
spinning machine used to achieve a flash heat process can
be a cotton candy type machine, such as the Econo-Floss*
Model 3017 manufactured by Gold Metal Products Company of
Cincinnati, Ohio. ,It will be appreciated by those skilled
in the art that any apparatus or physical process which
provides similar forcesand temperature gradient
conditions:can also be used. For simplicity in disclosing
and describing this invention, the terms "flash heat'~ will
be understood to mean a process which includes-subjecting
a feedstock to the combination of temperature, thermal
*Trade-mark
. J
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gradients, flow, flow rates, and mechanical forces of the
type produced in a cotton candy machine. The apparatus is
operated at the temperature and speed which permit flash-
flow of the feedstock without significant deterioration of
ingredients including, for example, a crystallization ,
control agent.
The matrix obtained in a melt-spinning process is in
the form of a floss, fiber, particle, flake, spicule or
any other generally non-descript amorphous aggregate.
Disclosures which relate to spinning substances with one
or more sugars are found in commonly-assigned U.S. Patent
NOS. 4,855,326, 4,8?3,085, 5,034,421, 4,99?,856,
5,028,632, 5,034,421 and 5,096,492. These disclosures
describe processing feedstock material by subjecting it to
high speed spinning on a spinning head in which the
substance is also subjected to heating against a heating
element.
Additional additives can be added to the matrix/oil
feedstock to achieve a variety of desired characteristics.
These include, without limitation, fillers, humectants,
emulsifiers, surfactants, coloring agents, flavors,
fragrances, sweetening agents, flash-flowable polymers,
plasticizers and the like.
As previously mentioned, the inventive delivery
system can be used.to provide enhanced flavor and/or
sweetness delivery due to the flavor oil being finely
dispersed in the sweetener matrix. The quality of the
flavor as well as the intensity is more predictably
released into the oral cavity due to the unique physical .
d
characteristics which are created during the flash-flow
process.
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By spinning the above-mentioned flavorant materials
with the soluble melt spinnable carriers, even normally
non-water soluble ingredients can be uniformly dispersed
when contacted with water. The formation of the matrix is
such that when added to a comestible such as chewing gum,
for example, the flavor materials carried in the matrix
rapidly dissolve when in contact with moisture. This
unique property results in a dramatic flavor impact in the
oral cavity.
In the case where two solid materials are to be used
as the matrix, they may be combined prior to melt-
spinning. For example, the matrix and the
organoleptically perceivable materials) may be combined
by co-crystallization. Co-crystallization involves
combining the ingredients in a heated state and thereafter
allowing them to cool in a unified, crystallized manner.
The unified structures are 'then reduced in size such as by
being ground before being spun.
Other means of combining organoleptic perceivable
materials with the matrix are also contemplated. For
example, the matrix and flavorant may be combined in the
spinning machine. In some cases, an oleaginous substance
such as corn oil or polyvinylpyrrolidone (PVP), can be
added to ensure uniform distribution of the flavor
dispersion throughout the matrix of the spun product. For
example, 2 parts oleaginous oil or a 2-3~ solution of PVF
may be added to the ingredients during the melt spinning.
The delivery system can also be compacted to less
than 50~ of the as-spun volume. Preferably, however, the
delivery system is compacted to less than 30~ and most
preferably to less than 15~ of the as-spun volume. As
previously mentioned, the delivery system may also be
reduced in particle size by milling before being added to
comestibles.
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The delivery system of the present invention has been
found to be especially effective as a dusting powder or
confectionery coating for chewing gum, confectioneries
tablets, nougats, dragies arid the like.
In the particular application with respect to chewing
gum compositions, the delivery system can be used as a
dusting powder on the surface of .the gum product. The
inventive powders have distinct advantages over dusting
powders conventionally used for a number of reasons. The
physical form of the inventive delivery systems allows for
immediate release of the flavor oil components when placed
in contact with the mouth. This has particular
significance in that up-front impact is achieved.
Additionally, due to the unique formulation of the oil
dispersion within the matrix, the intensity and quality of
the flavor can be more easily controlled. Furthermore,
the micronized flavor oil droplets within a sweetener
matrix gives the perception a fuller flavor with less
actual flavor being present. Since the delivery system
was formed using flash-flow processing, more flavor oil
components remain than with conventional simple mixing or
other encapsulation techniques. The sweetening agents
used as the matrix serve as anti-sticking or anti-blocking
agents during the gum making process, i.e., particularly
in the rolling and scoring pracess. a
The delivery system can be incorporated in
conventional chewing gum compositions. These compositions
typically contain a sweetener, a gum base and a flavor.
The sweetener generally also serves as a bulking agent in
sugared chewing gum compositions. One advantage of
employing the inventive delivery system in chewing gum
compositions is that the flavor can be directly ,
incorporated with the bulking agent rather than in a
separate step. Additional sources of flavor and/or
WO 93/08699 ' PGT/iJS92/094a7
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sweetener can of course be combined with the delivery
system arid incorporated in the chewing gum composition.
With regard to the chewing gum compositions, the
amount of gum base employed will vary greatly depending on
various factors such as the type of base, consistency
desired and other components used to make the final
product. In general, amounts of about 5~ to about 85~ by
weight of the final chewing gum composition are
acceptable, with amounts of about 15% to about 30'k by
weight being preferred. The gum base may be any water-
insoluble gum base well known in the art. Tllustrative
examples of suitable polymers in gum bases include both
natural and synthetic elastomers and rubbers. For
example, those polymers which are suitable in gum bases
include, without limitation, substances of vegetable
origin such as chicle, jelutong, gutta percha and crown
gum. Synthetic elastomers such as butadiene-styrene
copolymers, isobutylene-isoprene copolymers, polyethylene,
polyisobutylene, polyvinylacetate and mixtures thereof are
particularly useful.
The gum base composition may contain elastomer
solvents to aid in softening the rubber component. Such
elastomer solvents may comprise methyl, glycerol or
pentaerythritol esters of rosins or modified rosins, such
as hydrogenated, dimerized or polymerized rosins or
mixtures thereof. Examples of elastomer solvents suitable
for use herein include the pentaerythritol ester of
partially hydrogenated wood rosin, pentaerythritol ester
of wood rosin, glycerol ester of wood rosin, glycerol
ester of partially dimerized rosin, glycerol ester of
polymerized rosin, glycerol ester of tall oil rosin,
glycerol ester of wood rosin and partially hydrogenated
wood rosin and partially hydrogenated methyl ester of
rosin, such as polymers of alpha-pinene or beta-pinenet
terpene resins including polyterpene and mixtures thereof.
WO 93/a~699 PCT/US92/09447
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The solvent may be employed in an amount ranging from
about 10% to about 75% and preferably about 45% to about
70% by weight of the gum base.
A variety of traditional ingredients such as ;
plasticizers or softeners such as lanolin, stearic acid, '
i
sodium stearate, potassium stearate, glycerol triacetate,
glycerin and the like, including, natural waxes, such as
i
paraffin waxes and microcrystalline waxes may also be
incorporated into the gum base to obtain a variety of
desirable textures and consistency properties. In ;
accordance with the invention, however, these ingredients
may be reduced in amount or in some cases, may be
eliminated entirely. When present, these individual
additional materials are generally employed in amounts of
up to about 15% by weight and preferably in amounts of
from about 3% to about 10% by weight of the final gum base
composition.
The chewing gum may additionally include the
conventional additives of coloring agents such as titanium
dioxides emulsifiers such as lecithin and glycerol
monostearate; additional fillers such as aluminum
hydroxide, alumina, aluminum silicates; calcium carbonate;
and talc and combinations thereoft and additional
flavoring agents. These fillers may also be used in the
gum base in various amounts. Preferably, the amount of
fillers when used will vary from about ~% to about 35% by
weight of the final chewing gum.
The amount of delivery system used in the chewing gum
composition will largely be a matter of preference. It is .
contemplated that the delivery system will be included in
amounts of from about 0.25% to about 40% by weight of the ,
final gum compositian, with amounts of from about 1% to
about 30% being preferred, and amounts of from about 1% to
about 20% being most preferred.
WO 93/0699 ~'CT/L1592109447
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In addition to the invewtive 'delivery system, the
chewing gum composition may also optionally include one or
more additional ingredients such as conventional
polysaccharide-based bulking agents including sugars or
sugar alcohols, flavor delivery systems, spray-dried
flavors, liquid flavors, natural and/or artificial
sweeteners and the like.
3~n important feature o.f the chewing gum compositions
prepared in accordance with the present invention is the
l0 ability of the delivery system to rapidly dissolve when in
contact with the moisture present in tie oral cavity.
This feature significantly decreases the propensity of the
flavor ail to become entrapped arid solubilized within the
insoluble chewing gum cud during mastication.
The chewing gum compositions of the present invention
may be prepared by combining the water-insoluble gum base
portion and the water-soluble flavor portion including the
novel flavor/sweetener delivery system matrix according to
conventional chewing gum processing techniques.
For illustrative purposes, a method of preparing the
novel chewing gum compositions is as followss
A suitable chewing gum base is first melted.
Softeners and bulking agents such as sugar alcohols if
desired may be added slowly with stirring thereafter. The
inventive delivery system is then added and mixing is
continued until a homogeneous mass is achieved.
Optionally, additional flavor oils or spray dried flavors
may be added as well. The mass may then be rolled,
scored, dusted and wrapped in any manner known in the art.
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With regard to the preparation of other types of
comestibles, the spun matrix may also be added in a
conventional manner. For example, in the case of pressed
tablets, the flavor/sweetener delivery system may be dry
blended with the remaining tablet ingredi:ants and the
mixture thereafter compressed into final tablet form. In
the case of dentifrices, denture creams and cleansers, the
products also benefit from incorporation of the delivery
system in their formulations. In short, the matrix may be
a
added to various comestibles in a manner similar to that
which the skilled artisan currently uses to add
conventional water-soluble comestible ingredients.
The present invention also provides for enhanced
delivery of hydrophobic materials and allows these
materials which are normally difficult to disperse in
water, readily dispersible when placed in aqueous
solution.
The delivery systems of the present invention can
include a number of additional components which can be
dispersed along with the hydrophobic liquid. These
components can be pre-mixed with the liquid and added to
the feedstock mixture of matrix and oil, or added
concurrently with the matrix material and oil. For
example, various sweeteners, such as natural or synthetic
sweeteners can be combined with flavor oils by direct
addition or in spray-dried form. Additionally, the flavor
oil may be adsorbed on or incorporated in a carrier
material prior to admixture with the matrix materials.
Such carrier materials may include other flash-flowable
materials or may be materials which are not easily flash-
flow processed alone but can be added in amounts up to 50~
of the total composition arid combined with other more
flash-flowable materials.
W~ 93/08699 PCT/US9~/094d7
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In one particular embodiment, micron-sized sywthetic, '
i
amorphous silica has been used as a carrier for the
hydrophobic liquids. These silicas have a unique
combination of uniformity, chemical inertness, large
surface area and porosity which make them highly
adsorptive. These silicas can be manufactured with
precisely controlled surface area, porosity and particle
size distribution, which make them extremely useful in the
inventive compositions. Commercially available silicas of
this kind are sold under the trademarks SYLOID and SYLOX
by W.R. Grace & Co., Baltimore, MD. These materials are
specifically intended for use in dispersions and
suspensions. Using these materials, flavor oils can be
adsorbed onto their surfaces and into their pores and then
added to the feedstock of matrix material to form the
inventive delivery systems. In this manner, additional
controlled release characteristics can be imparted to the
delivery systems, as well as adding further stabilization
and protective features to the oils against volatilization
and oxidation. These silica compounds also have ionic and
hydrogen bond affinity far certain flavor component
chemical groups, which affinity serves to strengthen
flavor retention and consequently allows for increased
delayed release capabilities and stabilization
characteristics.
Additional materials which can be as carriers for the
flavor oils prior to incorporation with the inventive
delivery system include maltodextrins, such as spray-dried
maltodextrin marketed under the tradename M100 (10 DE) by
Grain Processing Corporation, Muscatine, IA, as well as
agglomerated maltodextrin (10 DE) sold under the tradename
Micropor Buds 1015A, by E. Staley Manufacturing Co.,
Decatur, IL. These materials are also porous and allow
for flavor retention. Polydextrose and microcrystalline
cellulose are also useful in this regard, as are a number
of other adsorbent materials.
WO 9310699 ~ ~ ~ ~ ~ 3 P~'/US92/09447
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Tn one embodiment, the sweetener matrix or other
matrix material can be combined with a cellulosic material
such as microcrystalline cellulose and flash-flow , I
processed. The resultant solid can then be further
processed in accordance with present invention by adding
artificial sweeteners and/or flavors and t:he like to it
and again flash-flow processed.
Microcrystalline cellulose can also xre used as the
primary matrix material and combined with natural or
ZO artificial sweeteners, such as those enumerated herein, to
form a delivery system which can be used °°as is" or
further combined with flavor oil and either flash-flow
processed further or added directly to a comestible or
other useful product, such as a pharmaceutical, cosmetic,
dry food or drink mix, cereal, personal hygiene product or
the like. '
V
The present delivery systems are also useful in
antacid compositions and especially those compositions
designed in chewable dosage forms. For example, these
compositions generally have sodium, calcium or magnesium
carbonates present and in some cases aluminum hydroxide.
The processes of the present invention have also been
shown to be especially useful in forming sweet and
flavorful products which have less sugar present. For
example, an artificial sweetener and/or flavor can be
combined with corn syrup solids as the matrix and flash-
flow processed with the inventive delivery system. The
delivery system can then be diluted with non-sweet fillers
such as starch or polydextrose and 'the like and added to
the final product, e.g. a comestible, thereby reducing the
amount of corn solids present in the final product.
'!3'O 93/0699 PC'T/LJS92/09447
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Invert sugar has also been found to be effective when
used in the present delivery system, especially in
combination with other flash-flavorable sweeteners because
it produces a product having less hygroscopicity. Other
materials which perform this function may also be used, as
well as materials which hold water well, such as
humectants, in applications where water content in the
processing or final delivery system is to be controlled.
E~iPLE~
The following examples serve to provide further
appreciation of the inventions but are not meant in any
way to restrict the effective scape of the invention.
Unless indicated otherwise, the Econo-Floss machine
referred to above was used to form delivery systems.
ER~1MFLE
Inventive delivery systems were prepared using
sucrose as the matrix and spearmint flavor oil as the
hydrophobic oil. In this example, 100 grams of sucrose
were first hand mixed with 2 grams of spearmint flavor oil
until a uniform mixture was obtained. The mixture was
then flash-flow processed at a medium setting arid
approximately 3500 RPM. The resultant delivery system
produced was a fine floss containing micronized droplets
of flavor oil which was thereafter milled to a particle
size of about 50 microns. The delivery system displayed
rapid solubility and high flavor impact when placed in the
mouth.
E~LE a
This example uses corn syrup solids as the matrix
material, along with orange flavor oil and corn oil. In
this example, 100 grams of corn syrup solids were hand
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7. y
mixed with 4 grams of orange flavor oil and 100 milligrams
of sucralose. Thereafter, 2 grams of Mazola~ corn oil was r
geometrically added to the mixture using a mortar and .
pestle. The mixture was then flash-flow processed at a
low setting to produce the inventive delivery systems
having a flake-like appearance and sweet, orangy taste.
E~MPLE 3
In this example, 100 grams of polydextrose K was hand
mixed with 100 milligrams of the artificial high intensity
sweetener sucralose until a uniform mixture was obtained.
Thereafter, 2 grams of Mazola~ corn oil was geometrically
added to the mixture using a mortar and pestle. The
resultant mixture was then flash-flaw processed at a law
setting to produce the inventive delivery system having a
chip-like appearance and intense sweetness.
In Examples 4-6, the delivery systems prepared in
Examples 1-3 are incorporated into chewing gum
compositions in the amounts set forth below. The
resultant chewing gum compositions display a rapid
perception of flavor with up-front high impact.
E~1MPLE 4
Chewing Gum
Ingredient Percentage by Weight
Delivery System (Example 1) 13.00
Gum Base 33.00
Carbohydrates 44.33
Softeners 9.50
Colorant 0.17
100.00
P~f/US92/094~17
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E~iFLE 5
Sugarless Che~rinc~ Gttm
Ingredient Percentage bY Weight
a
Delivery System (Example 2) 9.00
Gum Base 30.00
Carbohydrates 51.33
Softeners 9.50
Colorant _ 0-17
100.00
EJ~MI~LE 6
Sugarless Chewia a Gum
Ingredient Percentage by Weight
Delivery System (Example 3) 3.85
Gum Base 23.00
Carbohydrates 63.33
Softeners 9.50
Colorant 0.1?
Flavor Oil 0.15
100.00
In the following example, the delivery system of
Example 1 was included in a pressedtablet to demonstrate
that the soluble matrix also provides high flavor impact
in comestibles other than chewingums.
g
E~LAMPLS 7
Pr~ssed Tablets
Ingredient Percentage by Weight
Delivery System (Example 1) 22.00
Sugar 77.02
Copper Gluconate 0-75
(Breath Freshener)
Lubricant 0.23
100.00
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Examples 8 and 9 demonstrate the use of the novel
delivery systems in oral hygiene products. The high a
flavor impact provides an added organoleptic experience to ,
otherwise mundane daily routines.
EX~PSPLL 8
~'ooth Powder
Ingredient Percentage by Weight
Delivery System (Example 3) 2.40
Silica Hydrogel 95.10
Zinc Chloride 0.50
Sodium Fluoride 0.22
Sodium Gl.uconate 0.28
Sodium Methyl Cocoyltaurate 1.50
100.00
ExAMPLE '9
Dentifrice Composition
Tngredient Percentage by Weight
Delivery System (Example 2) 4.30
Glycerin 25.00
Silicone Dioxide 21.50
HMP (Hexaphos) 6.00
Silica 3.00
Sodium Lauryl Sulfate 120
Sodium Hydroxide (50~ solution) 1.0o
Xanthan Gum 1.00
Sodium Benzoate 0.50
Titanium Diaxide 0.50
Fluoride 0.22
Deionized Water Q.S. 100.00
!Va 93/0699 PCT/LJS92/09447
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Ep~,E ~~
This example is intended to demonstrate the use of
amorphous micron-sized silica as adsorbent carriers for
flavor oils which are incorporated into the inventive
delivery systems for the purpose of achieving delayed
release. A mixture of peppermint oil (75 gr.) and
amorphous silica (75 gr.) (SYL~OID 244 FP, Davison
Chemical) was mixed in a Hobart mixer. This mixture is
then added to polydextrose (2,348 gr.) and mixing is
continued. The mixture is then flash-flow processed on an
Econo-Floss spinning machine at 3600 RP~I at 190°C to yield
a fine flake-like material. This delivery system is then
incorporated in an amount of about 10% by weight into the
chewing gum composition of Examples 4 and 5, in place of
the delivery systems of Examples 1 and 2 respectively.
The resultant chewing gum products demonstrated a delayed .
flavor release due to the affinity of the flavor for the
silica and a reduced tendency of flavor oil to over-
plasticize the gum base.
E~MPhE 11
Examples 11 through 14 demonstrate the usefulness of
the inventive delivery systems as dusting powders on
chewing gum products, to aid in the rolling and scoring
processes and prevent sticking and binding in the overall
handling of the gum, both during processing and wrapping.
A flavor delivery system for delivery of up-front
flavor in the form of a powder is prepared for use on the
surface of a chewing product. 75 gr. of peppermint oil
was mixed with 75 gr. of SYLaID 244FP (obtained from
Davison Chemical) to which 1.5 gr. of aspartame and 0.5
gr» of saccharin were added followed by mixing. This
mixture was then gradually added to 2,348 gr. of
Palatinit~ Type PF (an isomalt obtained from SiaBungsmittel
i
1
WO 93108699 Pt'T/US92/09d~17
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209~~3 ~30-- -
GmbH, Manheim, Germany) in a Hobart mixer. The mixture
was then flash-flow processed on an Econo°Floss spinning
machine at 3600 RPM at 190°C yielding a white floss. The
material was cryoground with liquid nitrcigen to produce a
fine white powder.
The powder was applied to the surface of a chewing
gum mass which was then rolled between pxvassure rollers
and formed into a slab. The powder adhering to the gum
surface provided an immediate, pleasant sweet mint flavor
when placed on the tongue.
EBF~MPhE 12
The following flavor delivery system was prepared for
use on the surface of a chewing gum product. 10.0 gr. of
peppermint oil was mixed with 5.0 gr. of SYhUID 244FP to
which 1.0 gr. of flour salt was added followed by mixing.
This mixture was then gradually added to 394 gr. o:E
Sucrose 10x in a Hobart mixer. The mixture was then
flash-flow processed on an Econ-Floss spinning machine
(which was modified to provide variable speed control and
variable heat control) at 3,300 RPM at 190°C, yielding a
white floss. The material was cryoground with liquid
nitrogen to produce a fine white powder.
The powder was applied to the surface of a chewing
gum mass which was. then rolled between pressure rollers
and formed into a slab. The powder adhering to the gum
surface provided an immediate, pleasant sweet mint flavor
when placed on the tongue.
I;~IP~E 13
The following delivery system was prepared for use on
the surface of a chewing gum product. 1.6 gr. of
peppermint oil was mixed with 2 gr. of flour salt to which
dY0 93/~8699 1PGT/LT592/09447
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2.0 gr. of aspartame was added followed by mixing. 'this
mixture was then gradually added to 494.4 gr. of
polydextrose in a Hobart mixer. The mixture was then
flash-flow processed on an Econo-Floss spinning machine
(which was modified to provide variable s~>eed and variable
heat) at 3300 RPM at 140°C yielding a white floss. The
material was cryoground with liquid nitrogen to produce a
fine white powder.
The powder was applied to the surface of a chewing
gum mass which was then rolled between pressure rollers
and formed into a slab. The powder adhering to the gum
surface provided ar: immediate, pleasant sweet mint flavor
when placed on the tongue.
EBAMPLE 1~
The following flavor delivery system was prepared for .
use on the surface of a chewing gum product. 100 gr. of
peppermint oil was mixed with 5 gr. of SYT.~OID 244FP
(obtained from Davison Chemical) to which 1.0 gr. of flour
salt was added followed by mixing. This mixture was then
gradually added to 394 gr. of corn syrup solid PE 36
(obtained from Hubinger) in a Hobart mixer. The mixture
was then flash-flow processed on an Econo-Floss spinning
machine (which was modified to provide variable heat and
variable speed) at 3300 RPM at 145°C yielding a white
floss. The material was cryoground with liquid nitrogen
to produce a fine white powder.
The powder was applied to the surface of a chewing
gum mass which was then rolled between pressure rollers
and formed into a chewing gum piece. The powder adhering
to the gum surface provided an immediate, pleasant sweet
mint flavor when placed on the tongue.
'~O 93/08699 ;~ ~ ~ f;'~ PtC.'T/US92/09447
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The powders of Examples 1--4 can also be used to
provide up-front flavors bursts on mints, candies, baked
goods, dentifrices, pharmaceuticals and the like.
E~iPLP~~ 15 AND ~.6
The following delivery systems were made in
accordance with the process of the presenfi~ invention using
a spinning head temperature of about 140°C for Example 15
and 190°C for Example 16. Examples demonstrate the
physical form of the delivery systems to be a matrix
having a finely divided or micronized dispersion of flavor
droplets distributed therein.
Exrtm~le as
97% Maltrin - 365 (a maltodextrin DE 36)
3% Peppermint Oil
Examt~~.e 16
97~ Palatinit~ (an isomalt)
3% Peppermint Oil
The delivery system of Example 15 was then
photographed using conventional phase-contrast microscopy
techniques to clearly discern the oil phase from the
amorphous solid matrix. Figures 1 and 2 relate to Example
15, whereas Figures 3 and 4 relate to Example 16.
Figure 1 is a photomicrograph at 500x magnification.
The peppermint oil dispersion is clearly evident as those
areas where birefringence (double circle areas) is
present. The liquid can actually be seen to move within -
the encapsulated packet of the matrix and is easily w .
diseernable from air pockets, which lack both
birefringence and movement.
t
F~, W(~ 93/08699 ~'CT/US92/09447
°33° '
Figure 2 shows the delivery system of Example 15 at
1250x magnification subsequent to further cominution into
a powder by cryogrinding with nitrogen. The minute flavor
droplets are still present in the resultant powder, as
seen in the birefringent areas of the photomicrograph, as
well as through movement of the oil as seen under the
microscope.
Figure 3 is a photomicrograph (500x) of the delivery
system of Example 16. Again the flavor dispersion is
evident from the picture.
Figure ~ shows the same delivery system subsequent to
cryogrinding with nitrogen to a fine powder. The same
physical results are present, demonstrating that the
uniquely fine dispersion formed within the matrix remains
even after grinding.
ERA~iPLEE 1.7-19
These examples are intended to demonstrate the
ability of the inventive process and delivery system made
therefrom to better protect the volatile flavor
components.
A simple mixture of 92% Maltrin-365 (nE-36) and 8%
peppermint oil was prepared in a Hobart mixer. This
mixture was labelled Example 17. A sample of this mixture
was used as the feedstocl~ for preparing a delivery system
of the present invention using an Econo-Floss machine
(1~0°F, 3600 RPM). This delivery system was labelled
Example 18.
Finally, a sample of Example 18 was croground using
nitrogen and labelled Example 19.
WO 93/08699 PCfl~JS92/09447
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Each of Examples 17, 18 and 19 were incubated in a
temperature controlled environment (40°C) for an extended
period of time for the purpose of measuring volatile
component loss, or in other words, determining relative
flavor retention, Figure 5 graphically d~epic~ts the
j
percent oil remaining at various intervals of time. It is
abundantly clear from the graph that the inventive
delivery systems of the present invention (Examples 18 and
19) have retained the flavor over 168 hours at 40°C
significantly better than the simple mixture of Example
17. In fact, Example 18 shows only a nominal loss of
flavors as compared to the simple mixture of Example 17.
This is believed to be due to the unique physical
properties resulting from the novel form of the delivery
system.
While there have been described what are presently
believed to be the preferred embodiments of the present
invention, those skilled in the art will realize that
changes and modifications may be made thereto without
departing from the spirit of the invention, and it is
intended to claim all such changes and modifications as
fall within the true scope of the invention.
