Note: Descriptions are shown in the official language in which they were submitted.
~0~12
.
Description
Solid cssential Oil Flavor Composition
and Method of .~anufacture
Background of the Invention
The present invention relates to a
S process for producing a solid essential oil flavor
composition and the product of the process and
more particularly to such a process resulting in a
product in the form of a stable, extruded, solid
essential oil flavor composition.
ld
, .
- 15 In order to preserve the aroma and
flavor of various essential oils and make them
available for use in consumer products such as
beverages and the like, the prior art h~s
developed a n~mber of techniques for oroducing
solid essential oil compositions. These
compositions permit combination of the essential
oils into various products such as beverages to
which it is desirable to impart the aroma and
2--
flavor of the oil. Such techniques have been
found to be particularly useful and desirable, for
example, in connection with essential oils of
various citrus fruits while being equally useful
with essential oils from other sources. Citrus
fruit, for example, are characterized by essential
oils having particularly desirable characteristics
of aroma and flavor which are useful not only in
beverage products but in various food products as
lD well.
The prior art in this regard is
believed to be best exemplified by a number of
U. S. patents which are hereinafter discussed in
greater detail. These references include U. S.
Patents 2,809,895 and 3,041,180 issued
respectively on October 15, 1975 and June 2~, 1962
to H. E. Swisher under assignment to the assignee
of the present invention. The references also
include U. S. Patent 3,704,137 issued Novem~er 28,
1972 to Beck and U. S. Patent 4,271,202 issued
June 2, 1981 to Giel.
Turning now to these references, the
earlier Swisher patent disclosed a process for
forming solid essential oil flavoring composition
particles wherein an essential oil was emulsified
in hot corn syrup solids (42 DE) glycerine
solution, cooled, ground, rinsed with a solvent
and dried. The flavoring composition retained the
aroma and flavor of the oils within the particles
while making them available for release in various
consumer products such as beverages and other food
products.
The second Swisher patent disclosed an
improved process and solid essential oil flavoring
9~6~
~ --3--
.
composition wherein glycerine and corn syrup
solids ~42 DE) were formed into an aqueous,
semiplastic mass which was then combined with the
essential oil by means of an emulsifier, the
resulting combination being extruded into a cold
solvent to form an extruded solid wherein the
essential oil was encapsulated by khe glycerine
and corn syrup solids combination. This extruded
solid was then dried and an antica~ing agent
added, yielding an extruded particulate solid
having an extended shelf life while facilitating
its combination with beverage or other food
products to release the aroma and~or flavor of the
oil.
The Beck patent related to a similar
process and product as summarized above for the
second Swisher patent, except that the process and
product included a simple sugar and hydrolyzed
cereal solids ~less than 20 DE) with pyrogenic
~o silica as an anticakin~ agent.
The Giel patent related to a
spray-drying process for forming solid flavoring
` material capable of including high percentages of
flavoring oil per total particulate unit of
weight. Because of the high oil content possible,
such spray-dried products found wide use in a
number of beverages and other foods. However, it
was also found that spray-dried flavors typically
exhibit a relatively limited shelf life. In
addition, the high temperatures necessarily
involved during spray-drying processes have been
found to impair the flavor and aroma of various
heat-sensitive oil flavors, such as those in
citrus fruit. Furthermore, solids formed by
ï;~9c~6~2
.. ..
spray-drying commonly exhibit hygroscopic
characteristics making them difficult to handle
and store~
As noted above, spray dried oil flavors
have been used in the production of various
beverages and foods where it is desirable to take
advantage of their high oil content. At the sarne
time, extruded essential oil solids of the type
covere~ by the second Swisher and Beck patents
have also found a substantial market, particularly
where it is desirable to take advantage of the
better preserved aroma and flavor of the oil.
However, as was noted in the Beck patent, the
process for forming such extruded essential oil
flavor compositions has heretofore been considered
to have a practical maximum essential oil content
of about 12~ in the extruded particles. This
- limitation has at times prevented or limited the
use of extruded flavor compositions in certain
products where high oil content is desirable.
A number of patents issued to T. H.
Schultz, either alone or with other inventors,
including U. S. 2,856,291; 2,857,281; U. S.
2,899,313; U. S. 2,919,989; U. S. 2,929,72~ and
U. S. 2,929,723. Certain of these patents related
to processes for encapsulating essential oils in
generally the same manner as the Beck patent noted
above. In Schultz et al U. S. 2,857,281,
reference was made generally to use of an
essential oil or flavoring agent "to furnish about
from 5 to 25% thereof in the emulsion.~ However,
in the speci~ic discloses and examples provided in
the Schultz et al patent as well as in the other
patents where Schultz wàs an inventor, xesulting
~0~2
.
oil percentages in encapsulated form were far
- below the practical limit of 12~ noted above and
initially stated in the Beck patent.
Accordingly, there remains a need for a
process making possible the formation of stable,
extruded, solid essential oil or flavor
compositions having a relatively high percentage
- of essential oil encapsulated therein, preferably
at least in excess of the practical limit of 12%.
as stated in the Beck patent.
.Summary of the Invention
It is therefore an object of the
invention to provide an improved process for
forming an extruded, solid, essential oil flavor
composition and a product of such process while
. overcoming one or more problems of the type
summarized above.
It is a further object of the invention
to provide such a process for producing a
20 resulting product characterized by a ~elatively
high essential oi~ or oil-soluble flavor content
completely encapsulated within the extruded
particulate solids.
. It is an even further object of the
invention to provide such a process for producing
a resulting produc' charac~erized by a relatively
~ , .high essential oil or oil-soluble flavor content
: completely en~apsulated within the extruded
particulate solids.
~ 30 It is an even further object of the
invention to provide such a process for forming a
resulting product in the form of a stable,
melt-based and extruded, solid essential oil
1%9C)6~
--6--
flavor composition characterized by about 12 to
35% by weight of essential oil in substantially
completely encapsulated form within the extruded
solids. A somewhat hi~her percentage of the
essential oil or oil-soluble flavor is initially
added in the process to accommodate oil losses,
for example, during emulsification and solvent
washing of the product.
. It is a related object of the invention
to provide such a process for forming a resulting
product in the form of a stable, melt-based and
extrude~, solid essential oil flavor composition
- wherein a selected quantity of essential oil is
combined and blended with an aqueous mixture of a
sugar, starch hydrolysate and selected emulsifier
and at least preferably about 60% by weight, more
preferably 70~ by weight and most preferably about
75 to 80% by weight of the selected quantity of
essential oil is present in encapsulated form
within the resulting particulate essential oil
composition
Although, as noted above, the solid
essential oil flavor composition of the invention
~s preferably characterized generally by about 12
to 35% by weight of essential oil in substantially
completely encapsulated form, the present
invention more preferably contemplates the solid
: , essential oil flavor composition as being
characterized by about 14 to 30% by weight of
essential oil in substantially completely
encapsulated form within the extruded solids.
In accordance with the present
invention, it has been found that such a process
and product are possible by first forming an
. ,
.
9~;12
aqueous mixture of a sugar and starch hydrolysate
in combination with a suitable emulsifier, the
aqueous mixture and emulsifier is combined and
blended with a selected quantity of an essential
S oil or oil-soluble flavor in a closed vessel to
form a homogeneous melt under controlled pressure
conditions substantially greater than atmospheric
pressure.
It is an even further object of the
invention to provide such a process and product of
the process wherein the blending step is carried
out in a closed vessel pressurized within the
range of from about 7 to 50 pounds per square inch
~psi) or more.
It is yet a further related object of
the invention to cook the aqueous mixture of the
sugar and starch hydrolysate preferably to a
maximum temperature of about 126~ C before the
aqueous mixture and a selected emulsifier are
combined and blended with the essential oil in a
closed vessel as described above. More
preferably, the aqueous mixture is heated to a
maximum temperature of about 124 C and most
preferably to a temperature in the range of about
1~2 to 124 C generally under atmospheric ~ressure
conditions. These temperatures are especially
applicable where the essential oil comprises at
least about 28% by weight of the combination just
prior to emulsification.
A still further related object of the
invention is to carry out the heating step whereby
the resulting particulate essential oil
composition has a relatively higher water content,
preferably at least about 5% by weight.
.
.. ~ .
. ~ ~,'' .. .
. , . :
9~6~
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In connection with the present
invention, the term ~sugar" is intended to include
simple sugars such as sucrose, lactose, levulose,
dextrose, fructose and maltose, as well as polyols
such as glycerin and even other sweetners having
generally similar characteristics. Similarly, the
term ~starch hydrolysate" is intended to include
all hydrolyzed starches, both hydrolyzed cereal
solids of about 20 DE or less and corn syrup
solids of about 20 DE or higher. The term
"emulsifier" is used herein to indicate any
emulsifier which is satisfactory for use
particularly in combination with the selected
flavoring oil. Specific examples of suitable
emulsifiers are set forth within the following
detailed description. In addition, the term
"essential oil" is intended to include other oil
- soluble flavors which are capable of incorporation
in the process and product-of the present
invention.
Additional objects and advantages of
the invention are made apparent in the following
description having reference to the accompanying
drawings.
Brief Description of the Drawings
FIGURE l is a block-type flow sheet
including steps of the process of the present
invention and for forming the product of that
process.
FIGURE 2 is a graphic representation of
the effect of increased pressure on encapsulation
of the essential oil flavoring within the product
of the process.
~90~1~
.
Descxiption of the Preferred ~mbodiments
As noted above, the present invention
- relates to a process for forming or preparing a
stable, melt-based and extruded solid essential
oil flavor composition in particulate form as well
as the product of the proc:ess. Generally, the
process comprises the steps of (1) heating to a
suitable cook temperature an a~ueous mixture of a
sugar and a starch hydrolysate together with a
selected emulsifier, the cook temperature being
approximately the boiling point of the aqueous
mixture, 12) blending a selected quantity of an
essential oil flavor with the aqueous mixture to
form a homogeneous melt, (3) extruding the
1~ homogeneous melt into a relatively cool liguid
solvent to form extruded solids of selected size
and shape, and ~4) drying the particles and
blending with a selected antica~ing agent to
produce a stable and relatively non~hygroscopic
composition in particulate form. The process is
improved by the present invention in that the step
of blending or emulsifying the essential oil with
the aqueous mixture is carried out in a closed
vessel and the quantity of essen~ial oil flavor
added to the homogeneous melt is preferably
selected to provide about 12 to 35% by weight and
more preferably about 14 to 30~ by weight of
essential oil flavor in completely encapsulated
form within the particulate oil composition.
The present invention further
contemplates a process and product of the process
wherein preferably at least about 60~ by weight,
more preferably at least about 70% by weight and
~90~12
. --1 o--
most preferably at least about 75 to 8C~ by weight
of a selected quantity of e~sential oil combined
and blended with the aqueous mixture is present in
encapsulated ~orm within the resulting particulate
essential oil composition.
~ The invention also contemplates that
the sugar and starch hydrolysate, either together
with or pxior to combination of the selected
emulsifier therein, is preferably heated to a
maximum temperature of about 126 C in order to
minimize flavor deterioration of the essential oil
flavor and also to facilitate encapsulation
according to the present invention. More
pxeferably, the heating temperature is limited to
a maximum of about 12~ C and most preferably, th~
aqueous mixture is heated to a temperature in the
range of about 122 to 124 C generally under
atmospheric pressure conditions. These reduced
temperatures zre of greatest value when the
2~ essential oil comprises at least about 28% by
weight of the combination.
These temperature limits are discussed
in connection with the present invention in
greater detail below. In addition to minimizing
deterioration of flavor and other undesirable
characteristics of the essential oil which
commonly result at higher temperatures, the
reduced cook temperature is also believed to
permit a relatively increased amount of water to
remain in the melt prior to extrusion. It is
theorized that this additional water assists in
stabili2ing and facilitating emulsification and
encapsulation of the higher guantities of
essential oil within the particulate solid in
accordance with the process of the present
invention. Preferably, the invention contemplates
that the solid resulting from the,process of the
present invention comprise at least about 5~ by
w~ter.
At the same time, the above temperature
conditions for the heating step are preferably
stated as maximums at least within the broad and
preferred ranges since a number of variations in
the process may be carried out for accomplishing
similar results under even further reduced
temperatures. For example, it has been found that
a lower cook temperature may be used where a lower
DE rated sugar or sweetener is employed. For
example, if a 10 DE sweetener were employed in
place of the 20 DE sweetener described below in
connection with a number of examples, it would be
possible to urther reduce the cook temperature in
accordance with the present invention.
Similarly, it would also be possible to reduce the
cook temperature while otherwise achieving the
objects of the present invention by either
employing a greater degree of agitation during the
cooking process in order to facilitate removal of
excess water therefrom or by carrying out the
cooking process under vaeuum conditions for the
same purpose.
The second Swisher patent, and the Beck
patent referred to above discussed in substantial
detail the manner in which a homogeneous melt can
be formed from an aqueous mixture of a sugar and
starch hydrolysate together with a separate flavor
component to form an extruded solid capable of
being dried in the manner summarized above. Those
... .. .
6~LZ
.
references also discussed the manner in which such
a homogeneous melt can be extruded into a cool
liquid solvent to form particle of selected shape
and size as well as the selection of a suitable
~nticaking agent for combination with the extruded
solid particles in order to maintain them in a
more ~table condition. Accordingly, those
references are incorporated herein as though set
forth in full with respect to the particular
1~ features referred to above.
Referring now to the drawings and
particularly to FIGURE 1, a selected sugar and
starch hydrolysate are mixed together as indicated
at 12. The mixture is then agitated in order to
1~ uniformly mix together the sugar and starch
hydrolysate. As noted above, the sugar may be any
of the simple sugars such as sucrose, levulose,
dextrose, fructose or maltose, as well as a polyol
such as glycerine or other similar sweeteners.
Any preferred sugar or sweetner may be used for
any of a variety of reasons, such as to achieve
improved flavor of the resulting product and/or to
reduce hygroscopcity of the product. The mixture
12 is then heated to a coo~ temperature preferably
2i approximating its boiling point as indicated at
14. A suitable cook temperature ~or such mixtures
including most sugars extends across a range of
approximately 110 to 130~ C. For example, with
the sugar beiny sucrose and the starch hydrolysate
being 20 DE corn syrup, the boiling point of the
mixture is approximately 125-130 C and the
mixture is preferably heated to a temperature
within that range.
/ ~ ~
I
90~12
-13-
An emulsifying agent is preferablyadded to the a~ueous mixture 12 after the heating
step. Within FIGURE l, addition of the
emulsifying agent is indicated at 16; The
emulsifier is selected to facilitate
emulsification or dispersion of essential oil
described below into the mixture 14. Selection of
the particular emulsifier and the quantity of the
emulsifier added to the agueous mixture 14 is one
of the important features of the present invention
permit~ing from 12 to 35~ of a selected essential
` oil to be encapsulated within the final extruded
product. Suitable emulsifiers for use within the
present invention include sulfoacetate of mono-
and diglycerides as well as polyglycerol esters
and lecithin. Polyqlycerol esters suitable for
use within the present invention are available,
~or example, under the trademark identification
DREWPOL 6-2-S available from California Fats &
Oils, Richmond, California. Generally, the
polyglycerol esters have been found satisfactory
within the present invention for the lower end o~
the specified range.
One preferred emulsifier for
emulsifying and encapsulating up to 35~ essential
oil within the final extruded product is a
sulfoacetate of mono- and diglycerides containing
. 1% by weight water and available under the
trademark identification EMARGOL KL available from
the Witco Company. Emulsifiers such as those
referred to above are added to the molten mixture
14 in the amount of approximately 0.5 to 5% by
weight of the aqueous mixture. However, it is to
~e noted that the amount of emulsifier used in
l~g()~2
-such an application can vary depending upon other
factors. Accordingly, the above noted range is
set forth only as a general indication in
connection with the present invention~
Another emulsifier which has been found
to be particularly satis~actory in terms of the
present invention bu~ possibly less preferred than
the EMARGOL XL product rleferred to above is
lecithin, available for example from Ross & Rowe
under the trademark ~ELKIN TS.
Examples employing both of the
emulsifiers noted above are set forth below.
An essential oil or other oil-soluble
flavor contemplated for combination with the
mixture 14 and emulsifier 16 is generally
indicated at 18 and may be an essential oil, for
example, of a citrus fruit contemplated for use in
bever~ge or other food products.
The addition of a small amount of an
oil-soluble heat-stable antioxidant ~indicated at
20 in FIGU~E 1) such as 4-methyl-2, 6-ditertiary
butyl phenol or butylated hydroxyanisole is
optional. Generally, from about 0.05 to about
0.5~ by weight of the antioxidant, based on the
weight of the essential oil, is sufficient.
The essential oil 18, alone or in
com~ination with the antioxidant 20, is then added
to the a~ueous mixture 14 and emulsifier 16 in a
vessel 22. In accordance with the pr~sent
invention, it is particularly important that the
vessel 22 be closed during blending of the
essential oil 18 with the cooked aqueous mixture
14 and emulsifier 16. It has been found that the
carrying out of this blending or emulsification
~90~Z
-15-
step in a closed vessel is essential to insure
uniform and consistent encapsulation of relatively
large quantities of essential oil within the solid
product.
The closed vessel 22 is charged with
gas, preferably an inert gas such as nitrogen or
carbon dioxide, for example, to maximize
encapsulation of the oil or flavor. Even more
preferably, the vessel 22 is pressurized after
addition of the inert gas to a pressure from about
7 to 50 psi. In FIGU~E 1, addition of the inert
gas is generally indicated at 24. Pressurization
and its effects within the closed vessel 22 are
described in greater detail below with further
1~ reference to the graph of FIGURE 2.
Referring to FIG~RE 2, encapsulation of
substantially increased quantities of essential
oils or other oil-soluble flavors is illustrated
as being possible with pressurization in the
vessel 22 generally from about 7 to about 100 psi.
Destabilization of the resulting product sometimes
occurs with higher pressures at or above
approximately 100 psi. Best results are obtained
with the closed vessel 22 if pressure is
maintained within the approximate range of 7-50
psi.
In this regard, a pressure of about 7
psi is developed from vapor pressure alone
resulting from combination of the essential oil 18
with the molten mixture 14 and emulsifier 16
within the closed vessel. In such an event, the
vessel 22 is initially charged either with air or
an inert gas at atmospheric pressure.
~Z~9~6~-~
--lo--
Referring to FIGURE 2, the upper limit
of S0 psi for pressurization of the vessel 22 is
not a precise limit. In some applications, it is
possible to pressurize the vessel substantially
5 above 50 psi and even above 100 psi without
causing destabilization. ~owever, since the
amount of essential oil capable of encapsulation
within the final extruded product tends to
diminish when pressure is increased above 50 psi,
that pressure has been selected as the generally
preferred upper limit for pressurization of the
vessel 22.
Mixing of the essential oil 18, aqueous
mixture 14 and emulsifier 16 in the closed vessel
22 under pressure is continued until those
components are uniformly mixed and emulsified to
result in a homogeneous melt of the type also
discussed in the Beck and Swisher references, for
example. Generally, the homogeneous ~elt is
~efined as having a plastic condition suitable for
forming a solid product in the manner defined
below with an amphorous character for achieving
high stability over an extended period of time.
The homogeneous melt from the vessel 22
is then extruded under pressure, using either gas
or mechanical pressure, for example, into a cold
organic solvent such as isopropanol to form the
melt into extruded filaments.
Extrusion is carried out in an extruder
26 having die openings of a si~e selected in
accordance with the size and shape desired for the
- resulting particles. For example, where small
particles are desired for use in beverage or food
products, the homogeneous melt from the vessel 22
1~906~2
-17~
is extruded through openings (not shown) having
diameters, for example, of about l/32 inch.
Extruded filaments of the homogeneous
melt pass from the extruder 26 into a cold cold
organic solvent, such as isopropanol at about
-20 C, as generally indicated at 28. The
function of the isopropanol or other solvent is
two-fold. Initially, it acts as a coolant to
rapidly solidify the extruded shapes of
homogeneous melt. Secondly, it removes any
essential oil on the surface of the extruded
solids which would otherwise be susceptible to
oxidation. -
The extruded filaments are preferably
broken up into small rod-like particles while
within the solvent 28 in order to permit removal
of any essential oil exposed on the smaller or
separated particles. For example, the f ilaments
can be divided by impact action of an agitator
~o impeller ~not shown) to produce a desired particle
size and shape.
Following the solvent washing step 28,
the particles from the extruded filaments are then
screened or centrifuged at 30 to remQve the
organic solvent. The solvent is transferred to a
holding tank 32 and may be returned to the washing
step 28 if desired.
The particles from the separation step
30 are dried in a vacuum oven 33 and blended with
a suitable anticaking agent 36. The partlcles are
then screened by passage over a succession of
sizing screens (not shown) and packaged,
preferably in a dehumidified room, as indicated at
39~
l~g()~
1~-
The anticaking agent, as gen~rally
indicated at 36, is added to the particles after
drying to facilitate their urther handling and to
prevent the particles from sticking together. The
S anticaking agent is preferably silica, introduced
either before or after the particles are treated
- in the oven 33.
The process described above may be used
for preparing extruded solids containing essential
oils froln various sources. In particular, the
process of the invention is contemplated for use
in conjunction with various citrus fruits such as
oranges, grapefruit, lemons, etc. However, it
will be apparent that the process of the invention
is also useful with other essential oil or
oil-soluble flavors, either for use in beverages
or food products.
The product of the process described
above is novelly characterized as a stable,
melt based and extruded, solid essential oil
composition in particulate form. The particles
are of a solid amorphous character with a shape
determined by the extruder 26 and further divided,
for example, by impact breaking at 28. The
particles consist of a sugar and starch
hydrolysate as defined above, a selected
emulsifier and a selected essential oil flavor.
The essential oil flavor preferably forms about 12
to 35%, more preferably about 15 to 30%, by weight
of the particles while being present therein
completely encapsulated form.
The preceding process is particularly
adapted for assuring reproducible production of
particles having a high oil content as defined
.. . .. .
~9~z
-19-
above. ~he process is also particularly adapted
for forming about 12 to 35% by weight of the
particles with the essential oil flavor being
present therein in completely encapsulated form.
S The following examples of various
embodiments of the invention are presented to
further illustrate and exemplify but not to limit
the scope of the invention.
Exam~le 1
6025 grams of 20 DE corn syrup (70%
- solids), 4125 grams sugar and 200 grams EMARGOL RL
were mixed in a steam jacketed stainless steel
vessel. The vessel was fitted with a thermometer
and an agitator-assembly produced by C. E. Howard
Company, Los Angeles, California and having a flat
bladed turbine type agitator about 4 1/2 inches in
diameter. After heating to 130 during an initial
cook, 2200 grams of cold-pressed orange oil were
added to the vessel. The vessel was immediately
closed. After 5 minutes mixing with the aqitator,
the pressure inside the vessel had increased to 7
psi. During mixing, the cold-pressed orange oil
lowered the temperature of the aqueous mixture
below its cooking temperature, for example, to
about 125 C. After mixing was complete, nitrogen
was added to pressurize the vessel to 30 psi and
the melt was extruded through a plate with 0.030
inch diameter holes into 19 liters of cold
(-20~ C) isopropanol to solidify the filaments.
After impact breaking of the filaments, the
excess isopropanol was removed on a vacuum screen
and the material was dried for 3 hours in a vacuum
oven ~50D C, 27 in. Hg YacUUm). After addition of
0612
-20-
2% silica as an anticaking agent, the product
contained 16.7% by weight flavor.
Example 2
6025 grams of 20 DE corn syrup ~70~
solids), 4125 grams sugar and 200 grams EMARGOL KL
were mixed in a steam jacketed stainless steel
vessel. The vessel was fitted with an agitator
and thermometer as in Example 1. After heating to
130 C in an initial cook, 2200 grams of
cold-pressed orange oil were added to the vessel.
The vessel was immediately closed and pressurized
to 50 psi with nitrogen. After S minutes mixing
and agitation, the melt was extruded throuqh a
plate with 0.030 inch diameter holes into 19
l; liters of cold (-20 C) isopropanol to solidify
the filaments. The excess isopropanol was removed
on a vacuum screen and the material was dried for
3 hours in a vacuum over (50 C, 27 in Hg.
vacuum). After blending in 2~ silica, the product
contained 20.7% by weight flavor.
~xam~le 3
6025 grams of 20 DE corn syrup ~703
solids), 4125 grams sugar and 450 grams EM~RGOL KL
were mixed in a steam jacketed stainless steel
2~ vessel. The vessel was fitted with an agitator
and thermometer again as in Example 1. After
heating to 130 C in an initial cook, 2500 grams
of cold-pressed orange oil were added to the
vessel. The vessel was immediately closed and
pressurized to 50 psi with nitrogen. The melt was
then extruded through a plate with 0.030 inch
diameter holes into 19 liters of cold (-20 C)
~L~6~Z
isopropanol to solidify the filaments. The excess
isopropanol was removed on a vacuum screen and the
material was dried or 3 hours in a vacuum oven
(50~ C, 27 in. Hg. vacuum). After blending in 2%
silica, the product conta-ined 19.8~ by weight
flavor.
.. . ..
ExamDle 4
The steps of Example 3 were repea~ed
except that the vessel was pressurized to 100 psi
with nitrogen. Upon extrusion of the xesulting
product, the solids were found to be destahilized
as indicated at 38 in FIG~RE 2. Thus, Example 4
represents instability of the resulting product
upon pressurization to about 100 psi.
The steps of Examples 1-3 are also
capable of reproduction with other essential oils,
for example, from citrus fruit other than oranqes
or other oil-soluble flavors.
In addition, the steps of Example 1
were repeated with a number of other combinations
of essential oil and emulsifier as typified below
in Table I. Table I summarizes Examples 1-4 and
illustrates additional Examples 5-8 carried out
with the same steps and amounts described above
for Example 1 except where different amounts of
various components are indicated in Table I. As
noted above, about 7 psi pressure was developed
within the vessel 22 for each of these examples by
vapor pressure of the components being mixed
therein. At the same time, the temperature in the
vessel was reduced from the initial cook
temperature primarily by addition of the essential
oil to the cooked aqueous mixture.
96~61Z
--22--
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~ ~ O U~ O ' ~1 U~
H t~
~_I O o ~ ~ ~_ I` H ,~
t~ O
0 0
~ 0 ~ b ~
0
1~30612,
-~3-
The information set forth in Table I is
. .
summarized as follows. Initially, for Examples
5-8, the processing steps described in connection
with Example 1 were again followed including the
s identity and ~eight oE sugar and starch
hydrolysate. The amount of E~ARGOL KL and flavor
or essential oil is set fc)rth in Table I for each
of the examples. Also, the identity of the flavor
or essential oil for each of the examples is
ld indicated in the footnotes to Table I.
Thereater, the initial emulsifier content and
flavor or essential oil content are set forth as
percentages. These values were calculated based
- on the total weight of the product prior to
extrusion. Accordingly, the percentages are based
on a total weight of the sugar, starch
hydrolysate, emulsifier and flavor assuming loss
of all but about 5~ of the water from the corn
syrup or starch hydrolysate. Encapsulation
efficiency, referred to in the note following
Table I, was determined directly from the values
for initial flavor content and encapsulated
flavor. For example, encapsulation efficiency for
Example 1 was determined by dividing 16.7 by 20.1
and multiplying by 100 to result in encapsulation
efficiency of about 83.1%.
Information set forth below for
,. additional examples was determined in the same
manner described immediately above. It is again
noted that, for each of the examples, all but
about 5% by weight of the water from the starch
hydrolysate was removed during the initial cooking
step.
,~. .. , , . ~
~6~2
-2~-
Abbreviated data for Examples 9-13 is
set forth in Table II to demonstrate the efect of
coo~ temperature on encapsuLation efficiency. The
examples set forth in Table II were carried out in
the same pilot plant reactor used for each of
Examples 1-8. At the same time, each of Examples
9-13 was carried out according to the specific
steps set forth in connection with Example 6. The
only variation for Examples 9-13 was the heating
or cooking temperature to which the aqueous mix
was heated during the initial cook.
0612
-25-
qA3LE II
Encapsulation Efficiency vs. Cook Te~perature
OilEncapsulation Cook
mple No. caDsulatedEfficienc~le~perature, C
9 20.5 63.5 118
22.9 70.9 122
11 21.1 65.3 126
12 19.3 59.8 130
13 19.2 - 59.4 134
N'ote: In each of Examples 9-13, 6025 grams of 20 DE
oorn syrup ~70% solids), 4125 gra,~s sugar and 240 grams
EM~RGO~ KL were mixed in a steam jacketed stailless steel
vessel fitted with an agitator and thermometer as descri'ked for
preceding examples. ~le mixture was then heated to a cook
te~perature as set forth a'bove in Table II. Thereafter, 4200
grams of cold-pressed orange oil was added, the vessel
i,nmediately closed and agitation commenoed. A pressure of about
7 psi developed after about five nunutes of agitation m e
resulting melt was then extruded through a plate wit'n 0.030 inch
openings into 19 liters of cold (-20 C) isopropanol. The
solidified filaments ~ere im3act broken as described a'~ove,
excess isopropanol ren~ved b~ vacu~m, the material dried and
blen~ed with 2~ by ~eight silica. ~esulting encapsulating
efficienc~ for examples 9-13 is set forth in Table II.
. . .
~9[:)6~2
-26-
The data of Table II is set forth
: independently o~ the rest of the examples 9-13
- were all run at about the same time with the same
lots or batches of emulsifier, essential oil, etc.
Accordingly, Table II is believed to very clearly
~emonstrate a trend according to the present
invention in terms of encapsulation efficiency 2S
determined by the cook temperature.
At the same time, Examples 9-13
lG represent a relatively limited number of
temperatures in the range between 118 C and
135 C. Table III sets forth a larger number of
examples run in a similar manner as the examples
of Table II but at different times and possibly
with different lots of emulsifier, essential oil,
etc. Although the examples of Table III were run
in different equipment from those Table II, they
are believed sufficiently similar so that Tables
II and III taken together tend to establish the
~0 same trend, referred to above in connection with
Table II alone, as to the effect of cook
temperature on encapsulation efficiency according
to the invention.
~ Table III, below, sets forth Examples
14-39 which were also carried out in a similar
manner as described above for Examples 9-13 of
Table II. The examples of Table III were run ln a
large scale plant reactor rather than the pilot
plant reactor used in Table II. However, results
in Tables II and III are believed to be clearly
capable of corre9ation to further demonstrate
consistency for the process of the present
invention.
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t) ~1 r~ o a~ o 1-- 1~ o
L~ ~ .,
~ .
~ 'O ~ a~ ~ ~ ~ ~ ~1 ~ ~P O O O O ~
. .
a
~ O CO O ~ ~ ~ U~ ~ O ~ O ~3 0
H 1:~ ~
O ~ Ih u~ U~
a ~D ~ 00 CO C~ CO CO CO ~O ~ a~ ~ o o
.
o~ O O O G~ O O G~ o o o
.
`::
lZgO6~2
--28--
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,~ a~ ~ o cl~ 1-- ~ ~ s~ ~r ~ t~ er
dP ~ o u~ ~ O ~ ~ O~
~ ~3 .. ,
,~ ~a~ o co ,~ o ~
~ ~ ~ N 1~1 I~J ~1 ~ t`J ~ r~l _1
Q~
~ ~ ~ ~ ~`:1 N ~`1 ~I ~ ~ ~ r~
H
~P Q) tJ~
h
~1 ~J Q O a~ O O C~ O a~ O~ CO
.
~ o~ o~ o ~ ~ r~
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L2
, g
It may also be seen in connection with
Table III that unacceptable encapsulation
efficiency resulted particularly in connection
with Examples 26, 27, 38 and 39. Each of these
examples included a generally high cook
temperature varying from about 130 to about
134 C. In addition, those same examples included
relatively high initial essential oil contents
ranging from about 30.2 to about 32.9~ b weight.
Accordingly, Table III is believed to even further
emphasize the importance of cook temperature in
accordance with the present invention.
~ able IV, below, sets forth yet an
additional series of Examples 40-42, each carried
out using lecithin as an emulsifier.
~906~LZ
--30--
o' ~
~ o~
3 ~ a~ ~
~ . ..
.~
dQ rl ~ CO CO ~
o y ~ . ~
.~
~ o ~o ~
..... - ~
,,
O ~.~ ~ ~ ~D , .
N N CO
,~ .C ~
~ ~ ~ ~ a~ ~r
O ~I N
1~ ' .
-31-
: `
Table IV illustrates the ut~lity of the
present invention including lecithin as an
emulsifier. In each of Examples 40-42 of Table
IV, lecithin available from Ross & Rowe under the
tradename YELXIN TS was employed.
Table IV in particular demonstrates
that lecithin was quite effective as an emulsifier
where the essential oil WclS initially present in
an amount of about 22~ by weight. With an ini~ial
essential oil percentage of about 28, for example,
it is particularly important to employ a lower
cook temperature of no more than about 1~6 C and
preferably no more than about 123 to 124 C in
order to achieve effective encapsulation
efficiency.
Further Discussion of Prior Art
In order to further illustrate
advantages of the present invention, ~able V sets
forth Examples 43-51 only for the purpose of
20 representinq the ~rior art for pur~oses of
com~arison. Examples 43-51 were conducted in
essentially the same manner as Examples 9-13 of
Table II ~ut with the vessel remaining open during
mixing of the essential oil with the aqueous mix.
.
~ .
0~;12
--32--
g ~1 .
0 ~
O ~ o
~ ' ~ . ~ 0 ~o CO ~` ~ ~9
O ~ ~ co ~ c~ ~r ~ o ~ o
dP 0 U~ ~ O ~ O ~ ~ i o
-
cq 0 ~ ~D ~D ~ ~D ~ U~ C~ CO ~
~4 ,~
o
Z ~ ~ ~ r- co ~ o ,~
,,
,
~ ~ .
~ 9~ 2
-33-
Examples 43-51 are believed, by
contrast, to demonstrate further adv~ntages of the
present invention. A cursory review of Table V
indicates some high encapsulation efficiencies
S achieved even with an open mixing vessel, in
particular, Examples 43, 45 and 47. ~owever, it
is especially important to note that the initial
amount of essential oil employed in each of
Examples 43-Sl.was very lo~ compared to that in
Examples 1-42.
Even with the advantage of lower
initial oil content, encapsulation efficiency was
not repeatable even for the limited purpose of
~ccomplishing uniform encapsulation with oil
content in the range of about 12 to 15%. ~or
example, note that whereas Example 43 resulted n
encapsulation efficiency of 90%, substantially
identical Example 44 resulted only in
encapsulation efficiency of 66% with an oil
:20 content in encapsulated form of only 10.8%. The
other examples of Table V demonstrate similar
inconsistent results and thus are believed to
further assist in emphasizing the novel features
of the present invention.
In view of the preceding description
and Examples 1-42, other modifications of the
process and resulting product of the present
invention, in addition to those noted above, will
be apparent to those skilled in the art.
Accordingly, the scope of the present invention is
defined only by the following appended claims.
