U.S. patent application number 09/540383 was filed with the patent office on 2002-05-30 for long flavor duration releasing structures for chewing gum.
Invention is credited to MAXWELL, JAMES R., SONG, JOO H., TOWNSEND, DONALD J..
Application Number | 20020064576 09/540383 |
Document ID | / |
Family ID | 22430124 |
Filed Date | 2002-05-30 |
United States Patent
Application |
20020064576 |
Kind Code |
A1 |
SONG, JOO H. ; et
al. |
May 30, 2002 |
Long flavor duration releasing structures for chewing gum
Abstract
The present invention provides methods and compositions for
improving the flavor duration in chewing gum. In a preferred form,
the present invention provides matrix compositions comprising a
hydroxypropylcellulose cross-linked with a multi-functional
carboxylate to yield a matrix having a lower water solubility than
the original cellulosic material. This matrix may be ground up,
have a flavor incorporated therein and used in gum compositions in
which it facilitates a prolonged release of the flavoring.
Inventors: |
SONG, JOO H.; (CHICAGO,
IL) ; TOWNSEND, DONALD J.; (MOORES HILL, IN) ;
MAXWELL, JAMES R.; (CHICAGO, IL) |
Correspondence
Address: |
BRINKS HOFER GILSON & LIONE
P.O. BOX 10395
CHICAGO
IL
60610
US
|
Family ID: |
22430124 |
Appl. No.: |
09/540383 |
Filed: |
March 31, 2000 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
|
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60127439 |
Apr 1, 1999 |
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Current U.S.
Class: |
426/3 |
Current CPC
Class: |
A23G 4/06 20130101; A23G
3/346 20130101; A23G 3/346 20130101; A23G 2220/02 20130101; A23G
2200/14 20130101; A23L 27/70 20160801; A23G 3/346 20130101; A23G
4/10 20130101; A23G 4/20 20130101; A23G 2200/14 20130101; A23G
2220/02 20130101; A23G 4/02 20130101 |
Class at
Publication: |
426/3 |
International
Class: |
A23G 003/30 |
Claims
1. A method of making a long flavor duration releasing structure
for chewing gum comprising: a) mixing a cellulose material having
hydroxyl groups thereon with a multi-functional carboxylate to form
a generally homogeneous composition; b) treating the composition to
a curing temperature for a sufficient amount of time to form a
matrix having a low water solubility; c) sizing the matrix to a
size to be used in chewing gum compositions; and d) incorporating
flavoring agents into the matrix.
2. The method of claim 1 wherein the sizing step is performed by
grinding the matrix.
3. The method of claim 1 wherein the step of incorporating flavor
into the matrix occurs after the step of sizing the matrix.
4. The method of claim 1 wherein the cellulose material comprises
hydroxypropylcellulose.
5. The method of claim 1 wherein the multi-functional carboxylate
is selected from the group consisting of sodium
carboxymethylcellulose, adipic acid, malic acid, citric acid and
mixtures thereof.
6. The method of claim 4 wherein the multi-functional carboxylate
comprises sodium carboxymethylcellulose.
7. The method of claim 1 wherein the cellulose material has an
average molecular weight of between about 80,000 and about
1,150,000.
8. The method of claim 1 wherein the ratio of cellulose material to
multi-functional carboxylate is between about 99:1 and about
9:1.
9. The method of claim 6 wherein the ratio of
hydroxypropylcellulose to sodium carboxymethylcellulose is about
95:5.
10. The method of claim 1 wherein the step of mixing includes
distributing the cellulose material and the multi-functional
carboxylate in a liquid medium.
11. The method of claim 1 wherein the step of mixing includes
dissolving the cellulose material and the multi-functional
carboxylate in an aqueous solution.
12. The method of claim 6 wherein the hydroxypropylcellulose and
sodium carboxymethylcellulose are each dissolved in water before
being mixed together.
13. The method of claim 1 wherein the step of mixing includes
making a solution containing between about 1% and about 10%
hydroxypropylcellulose, between about 0.1% and about 1.0% sodium
carboxymethylcellulose, and between about 98.9% and about 89%
water.
14. The method of claim 1 wherein the step of mixing includes
blending the cellulose material and the multi-functional
carboxylate together in a dry state and then dissolving the mixture
in an aqueous solution.
15. The method of claim 1 wherein the composition is cured at a
temperature of at least 120.degree. C. for a period of at least 4
hours.
16. The method of claim 1 wherein the composition is cured at a
temperature of between about 120.degree. C. and about 250.degree.
C.
17. The method of claim 1 wherein the composition is cured for a
period of between about 4 and about 48 hours.
18. The method of claim 1 wherein the composition is cured for a
period of at least 8 hours at a temperature of at least 135.degree.
C.
19. The method of claim 1 wherein composition is dried in a forced
air oven at a temperature of between about 20.degree. C. and about
40.degree. C. before being cured.
20. The method of claim 1 wherein the composition before curing
comprises between about 0.5% and about 5% water.
21. The method of claim 1 wherein the matrix is ground to a size of
less than 20 mesh.
22. The method of claim 1 wherein the flavoring agent is
incorporated into the matrix at a ratio of between about 0.05 and
about 1 part flavoring agent to 1 part matrix.
23. The method of claim 1 wherein the flavoring agent is
incorporated into the matrix at a ratio of about 2 parts matrix to
1 part flavoring agent.
24. The method of claim 1 wherein the composition is made in an
extruder and cured thereafter.
25. The method of claim 24 wherein a lubricant is added to the
composition to aid in the extrusion process.
26. The method of claim 25 wherein the lubricant is selected from
the group consisting of water, alcohol and mixtures thereof.
27. A long flavor duration releasing structure comprising: a) a
cellulose material with hydroxyl groups thereon mixed with a
cross-linking agent and cured to form a matrix having a low water
solubility, and b) a flavoring agent incorporated into the
matrix.
28. The long flavor duration releasing structure of claim 27
wherein the cross-linking agent comprising a multi-functional
carboxylate.
29. The long flavor duration releasing structure of claim 28
wherein some of the hydroxyl groups react with the multi-functional
carboxylate to make cross-links.
30. A chewing gum composition with long flavor duration comprising:
a) a gum base; b) a water soluble bulk portion; and c) a flavor
releasing structure comprising: i) a matrix formed by mixing an
aqueous solution containing hydroxypropylcellulose with an aqueous
solution containing a cross-linking agent and evaporating water
from the mixture; and ii) a flavor agent incorporated into the
matrix.
31. The chewing gum composition of claim 30 wherein the
cross-linking agent comprises sodium carboxymethylcellulose.
32. The chewing gum composition of claim 30 wherein the flavor
releasing structure causes the flavoring agent to be released upon
chewing the gum generally during the time period between about 5
minutes after chewing begins and about 15 minutes after chewing
begins.
33. The chewing gum composition of claim 30 wherein flavor
releasing structure comprises between about 0.1% and about 5% of
the gum composition.
34. A method of making a chewing gum composition with a long flavor
duration comprising the steps of: a) mixing a cellulose material
having hydroxyl groups thereon with water until the cellulose
material is hydrated; b) drying the water from the cellulose
material; c) curing the cellulose material for a time period of at
least 6 hours and at a temperature of at least 125.degree. C. to
form a matrix having a lower water solubility than the original
cellulosic material; d) sizing the matrix to a size useful as an
ingredient in chewing gum; e) incorporating flavor into the matrix;
and f) mixing the matrix with flavor incorporated therein with a
gum base and a bulking agent to form the chewing gum composition.
Description
REFERENCE TO EARLIER FILED APPLICATION
[0001] The present application claims the benefit of the filing
date under 35 U.S.C. .sctn. 119(e) of provisional U.S. patent
application Ser. No. 60/127,439, filed Apr. 1, 1999, which is
hereby incorporated by reference.
FIELD OF THE INVENTION
[0002] The present invention relates to flavoring of chewing gum.
More particularly, the present invention describes methods and
compositions for providing a long flavor duration in chewing
gum.
BACKGROUND OF THE INVENTION
[0003] Chewing gums typically contain many ingredients including
flavor ingredients, sweetener ingredients and flavor-enhancing
ingredients. It is often desirable to produce a chewing gum having
a high degree of sweetness and flavor, which lasts for an extended
period of time. "Fast release" chewing gums known in the art
typically release their flavor and sweetness compounds rapidly,
creating an initial burst of high intensity sweetness and flavor
which is pleasing to the consumer but which does not last.
Conversely, "slow-release" chewing gums release their sweetness and
flavor over a longer period of time but do not provide an initial
burst of high intensity sweetness and flavor. Hence, chewing gum
manufacturers are constantly trying to extend the time in which
consumers can enjoy the sweetness and flavor of chewing gum without
sacrificing the quality of the initial sweetness and flavor
impact.
[0004] Various methods and compositions have been described for
providing better control of the release of flavoring agents and
increasing the length of flavor duration. For example the art
describes the encapsulation of flavoring agents and other active
ingredients into matrices. Examples of such matrices are disclosed
in, for example, U.S. Pat. Nos. 4,978,537; 2,290,120; 2,596,852;
3,085,048; 3,795,744; 3,826,847; 3,818,107; 3,962,463; 4,217,368;
4,259,355; 3,962,463; 4,217,368; 4,259,355; 4,230,687; 4,590,075
and 5,128,155 and PCT Patent Publication No. WO 98/27826 (each of
which is incorporated herein by reference). These patents are
discussed in further detail herein below.
[0005] U.S. Pat. No. 4,978,537 discloses gradual release structures
formed by meltspinning a mixture of an active agent and a wall
material. U.S. Pat. No. 2,290,120, discloses the mixing of
particles of chewing gum base with the flavoring agent to provide a
substantially homogeneous mixture.
[0006] U.S. Pat. No. 2,596,852 discloses chemically reacting the
chewing gum base with molecules of flavor ingredient, wherein the
chewing gum base is a vinyl acetate polymer and the flavor molecule
contains an ethylenic bond. U.S. Pat. No. 2,886,446, discloses the
coacervation of a typically volatile, water immiscible flavoring
oil within a body of gelatin. U.S. Pat. No. 3,085,048 discloses a
process for coating dicalcium phosphate with sugar. U.S. Pat. Nos.
3,795,744, and 3,826,847 disclose the coating, encapsulation or
combination of flavoring agents with high molecular weight
compounds including starches, cellulose, proteins, gums, polyvinyl
alcohol and polyvinyl esters. U.S. Pat. No. 3,818,107, discloses
flavoring agent appended to a polymer backbone, releasable upon
hydrolysis.
[0007] U.S. Pat. No. 3,962,463 discloses the encapsulation of
flavor ingredients in gelatin waxes, polyethylene and the like
followed by the depositing of the encapsulated flavor particles on
the surface of the chewing gum. U.S. Pat. No. 4,217,368 discloses
the controlled release of a (second) sweetener which is dispersed
in, enveloped by, trapped in and otherwise protected by the gum
base. A first sweetener, which is relatively unprotected, provides
an initial burst of flavor. U.S. Pat. No. 4,259,355 discloses a
hydrolytically releasable flavor oil entrapped in gelatine,
dextrin, gum acacia or modified food starch with the aid of a
hydroxypropylcellulose solid suspending agent. A hydrophobic
unconfined flavor oil provides an initial burst of flavor.
[0008] U.S. Pat. No. 4,230,687 discloses the encapsulation of
flavoring agent in a polymeric medium using rigorous and intimate
conditions of mechanical shear to mix the flavoring agent with the
encapsulating medium. The flavoring agent is gradually released
from the encapsulating matrix at a rate dependent upon the rate of
hydration of the matrix, which in turn depends upon the particular
matrix used. The polymeric matrix may be derived from natural
substances such as casein, a gelatin, modified starches, gums and
related materials.
[0009] U.S. Pat. No. 4,590,075 discloses a flavor and sweetener
delivery system including a flavoring agent and/or sweetener
encapsulated in an elastomeric matrix. The elastomeric matrix is
substantially hydrophobic and includes an elastomer, an elastomer
solvent, a wax system and an excipient. The excipient, which is
present only in small amounts, can include carbohydrate materials
(including partially hydrolyzed starch), polyhydric alcohols, and
mixtures of carbohydrates and polyhydric alcohols.
[0010] Despite this substantial body of work, there remains a
deficiency in the art in that the duration and intensity of flavor
can not be sustained for long periods of time. A matrix material
that has attracted interest for its ability to improve flavor
characteristics of gum is hydroxypropylcellulose (hereinafter
referred to as HPC). U.S. Pat. No. 5,128,155 (specifically
incorporated herein by reference) describes HPC compositions with
silica and plasticizers as flavor cores for chewing gum. In these
compositions, the silica was thought to be necessary and sufficient
to act as a flavor reservoir material. PCT Publication WO 98/27826
suggests that low levels of HPC may be useful in increasing the
amount of flavor released from chewing gum. For these compositions
to be useful it was necessary to incorporate the HPC directly into
the gum composition, as opposed to being premixed with another
ingredient or used as an encapsulant or agglomeration agent.
Furthermore, the HPC had to be present in concentrations of less
than 1% if the gum integrity was to be maintained.
[0011] Clearly, the prior art demonstrates that there is a need for
increasing the flavor duration and intensity in chewing gum
compositions. While this need has been partly met, further
improvements would be a great benefit. The present invention is
directed toward methods and compositions overcome this deficiency
in the prior art.
BRIEF SUMMARY OF THE INVENTION
[0012] There is a need in the art to improve the flavor duration
and/or intensity of chewing gum. The present invention is directed
towards addressing this need. The present invention provides
methods and compositions that improve the duration of flavor in
chewing gum without compromising the integrity of said gum or
flavor. This beneficial outcome is preferably achieved by using
novel high molecular weight HPC matrices.
[0013] In particular, the present invention provide a method of
making a long flavor duration releasing structure for chewing gum
comprising mixing a cellulose material having hydroxyl groups
thereon with a multi-functional carboxylate to form a generally
homogeneous composition; treating the composition to a curing
temperature for a sufficient amount of time to form a matrix having
a low water solubility; sizing the matrix to a size to be used in
chewing gum compositions; and incorporating flavoring agents into
the matrix.
[0014] Other aspects of the present invention provides a long
flavor duration releasing structure comprising a cellulose material
with hydroxyl groups thereon mixed with a cross-linking agent and
cured to form a matrix having a low water solubility, and a
flavoring agent incorporated into the matrix.
[0015] Also contemplated herein is a chewing gum composition with
long flavor duration comprising a gum base; a water soluble bulk
portion; and a flavor releasing structure comprising:
[0016] i) a matrix formed by mixing an aqueous solution containing
hydroxypropylcellulose with an aqueous solution containing a
cross-linking agent and evaporating water from the mixture; and
[0017] ii) a flavor agent incorporated into the matrix.
[0018] Yet another aspect of the present invention provides a
method of making a chewing gum composition with a long flavor
duration comprising the steps of mixing a cellulose material having
hydroxyl groups thereon with water until the cellulose material is
hydrated; drying the water from the cellulose material; curing the
cellulose material for a time period of at least 4 hours and at a
temperature of at least 120.degree. C. to form a matrix having a
lower water solubility than the original cellulosic material;
sizing the matrix to a size useful as an ingredient in chewing gum;
incorporating flavor into the matrix; and mixing the matrix with
flavor incorporated therein with a gum base and a bulking agent to
form the chewing gum composition.
[0019] Other objects, features and advantages of the present
invention will become apparent from the following detailed
description. It should be understood, however, that the detailed
description and the specific examples, while indicating preferred
embodiments of the invention, are given by way of illustration
only, since various changes and modifications within the spirit and
scope of the invention will become apparent to those skilled in the
art from this detailed description.
BRIEF DESCRIPTION OF THE DRAWING
[0020] The following drawing forms part of the present
specification and is included to further demonstrate certain
aspects of the present invention. The invention may be better
understood by reference to this drawing in combination with the
detailed description of specific embodiments presented herein.
[0021] FIG. 1 is a graph comparing flavor intensity throughout most
of the chewing period for the preferred matrix of the present
invention and previously made flavored cores.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS OF THE
INVENTION
[0022] There is a need in the art to provide methods and
compositions for increasing the duration and intensity of flavor in
chewing gum. The present invention addresses this need by providing
methods and compositions that prolong the flavor duration of
chewing gum. More particularly, the inventors have demonstrated
that it is possible to produce a long flavor duration releasing
structure by preparing a homogeneous composition of a
hydroxycellulose material with a multi-functional carboxylate and
mixing the two ingredients in water, blending, drying, and curing
the composition to form a matrix that has a low water solubility.
This matrix can then sized and flavored as desired. The methods and
compositions for producing this beneficial matrix are described in
greater detail herein below.
[0023] As used herein, the term "curing" means treating the
composition to sufficiently high temperatures to allow the
composition to adopt a solid configuration that can be ground. In
order to test whether the matrix composition has been sufficiently
cured, a "wet finger" test can be performed. If the cured
composition is wetted on the fingers and the matrix appears to
dissolve and give a wet, slimy feel, the composition has not been
fully cured. If the matrix is properly cured, it will not
appreciably dissolve in water, nor will a slimy film form when
handling the matrix with wet fingers. Such a suitably cured
composition is said to have a "low water solubility" as used
herein. The following description provides exemplary matrix
components, flavorings and other gum components, and methods of
producing the cured matrix and using it in the manufacture of
chewing gum compositions.
[0024] Matrix Components
[0025] The present invention provides methods and compositions
relating to improved flavor duration in chewing gum. The inventors
have found that using a hydroxycellulose, and more particularly
HPC, in flavor cores improves the duration of flavor in chewing
gum. Previous flavor cores used HPC with silica and plasticizers to
make the flavor cores. High MW HPC gave longer flavor duration and
low MW HPC gave short flavor duration. High MW HPC materials also
gave a narrow release time with a strong release of flavor.
However, at high usage levels in the gum, the HPC materials caused
the gum to have a slimy texture. As a result, the amount of flavor
which could be added to the gum using these cores had a practical
limit. An even higher MW HPC for even longer flavor duration would
be desired, but this type of material is not available as a food
grade product. A mixture of HPC and sodium carboxymethyl cellulose
(hereafter referred to as sodium CMC) when dried and cured was
found to give a new matrix material. When flavor was absorbed onto
this matrix material, the material gave a good, broad flavor
profile, and a longer duration time. Also there was no slimy
texture when flavor was released as with the high levels of the
previous high MW HPC.
[0026] The HPC/CMC matrix formed by the process noted below may or
may not be a cross-linked material. The matrix may be due to a
physical phenomenon or may be cross-linked. Analysis of the matrix
by various methods has not demonstrated that the matrix is
cross-linked. However, cross-linking may be very insensitive to
these analysis and the cross-linking level may be too low to be
detected. Also, any cross-linking may be breaking down during
analysis of the matrix or during its shelf life. The analysis may
actually be of the breakdown products which are HPC and sodium CMC.
In theory, the HPC and sodium CMC materials may be cross-linked to
give this newly structured matrix. This matrix can give the
properties of a very high molecular weight HPC and modify the
flavor profile and delay release.
[0027] A maximum level of about 5% to about 10% by weight of sodium
CMC to about 90% to about 95% HPC should be sufficient to obtain
the new product matrix. Generally, the matrix may be formed by
mixing the two ingredients in water, blending, drying, and curing
at high temperature. To expedite production for full scale
production of this matrix, the matrix may be extruded, since this
would give faster drying and allow for faster and easier
manufacture. In this case, the matrix ingredients may be blended
with a lubricant such as water, alcohol, and mixtures thereof. The
following section provides a more detailed discussion of the matrix
components and production.
[0028] a. HPC
[0029] In specific embodiments of the present invention
hydroxycellulose compositions are employed as part of a matrix core
to form flavor reservoirs. An exemplary cellulosic material that is
preferred for this purpose is cellulose 2-hydroxypropyl ether,
which is called hydroxypropylcellulose. This material is sold by
Aqualon Co., a subsidiary of Hercules Inc., under the trademark
Klucel.RTM..
[0030] Hydroxypropylcellulose is available in different molecular
weights. Varying the molecular weight may affect the release
characteristics of the cores. For example, Klucel HF has a
molecular weight of about 1,150,000 and Klucel EF has a molecular
weight of about 80,000. Thus, it will be possible to chose HPC
compositions that will produce high or very high MW matrices when
cross-linked or treated according to the methods of the present
invention.
[0031] Although HPC is the preferred cellulosic material for use in
the present invention, it is contemplated that other cellulosic
materials also will be useful. Various grades of HPC are
commercially available to those of skill in the art, for example,
Klucel HFF is food-grade and Klucel HF is cosmetic grade. Preferred
embodiments employ Klucel HFF.
[0032] In preferred embodiments, the present invention provides an
HPC matrix for use as a flavor duration enhancer in chewing gum
compositions. In particularly preferred embodiments, the chewing
gum composition comprise between about 0. 1% to about 4% HPC. In
specific embodiments, it is contemplated that the HPC content of
the chewing gum composition may be about 1.98%. Of course it is
contemplated that the HPC content of the chewing gum composition
may of any other range such as between about 0.5% to about 2%;
between about 0.75% to about 1.5%; and between about 1% to about 2%
of the chewing gum composition. It is of interest to note that in
the prior art a 1% HPC content in gums resulted in a loss of
integrity of the gum composition (WO 98/27826). It has previously
been noted that the presence of 1% HPC resulted in a gum with an
undesirable slimy texture.
[0033] b. Sodium CMC
[0034] To form a cross-linked HPC matrix, a small amount of a
cross-linking agent is needed; this cross-linking agent preferably
is a multi-functional carboxylate. As used herein the term
"multi-functional carboxylate" refers to a compound that contains
two or more carboxylic acid moieties or salts thereof.
[0035] The carboxyl groups react with the hydroxyl groups from HPC
and when water is removed may give a cross-linked HPC. Although it
is desirable that sodium CMC is used as the cross-linking agent,
other types of materials such as various organic acids also may be
effective as cross-linking agents. Indeed it may be that in the
curing process employed herein, the HPC may be able to cross-link
with itself forming HPC multimers and thereby forming a matrix
without the need for additional cross-linkers.
[0036] As is well known, sodium CMC has long been manufactured in
industry and has been applied in a variety of uses, such as paste
or thickening agent. Such uses for sodium CMC are well known to
those of skill in the art and are described in for example, U.S.
Pat. Nos. 4,063,018; 4,883,537 and 4,525,585 (each incorporated
herein by reference).
[0037] In addition to sodium CMC, other multi-functional
carboxylate groups include but are not limited to adipic acid,
malic acid, citric acid and the like. Of course, mixtures of these
acids also may be employed. It is understood that it will be
necessary to ensure that the multi-functional carboxylate
composition is of a food-grade quality. Food-grade sodium CMC is
readily available and well known to those of skill in the art. A
particularly preferred sodium CMC is type 7H3SF which is available
from by Aqualon Co., a subsidiary of Hercules Inc.
[0038] In preparing the matrix of the present invention, it is
contemplated that the sodium CMC (or other cross-linking agent) may
comprise between about 1% up to about 10% of the matrix relative to
the HPC content. It is therefore contemplated that the composition
certain embodiments may comprise any range of sodium CMC
concentration between this range, thus in certain embodiments the
sodium CMC concentration may be between about 2% and about 8%; in
other embodiments the range may be between about 4% and about 6%,
in particularly preferred embodiments the sodium CMC content is 5%
of the matrix composition relative to the HPC content of the
composition.
[0039] c. Preparation of the Matrix
[0040] It is believed that the following process gives a
cross-linked HPC/CMC matrix, but there is the possibility that
instead of cross-linked product, the process may just give a matrix
with a mixture that gives the desired physical properties possibly
due to hydrogen bonding.
[0041] In an exemplary embodiment presented herein, the matrix is
prepared by adding a solution containing 11.35 g sodium CMC to a
solution containing 215.65 grams of high molecular weight HPC. The
HPC is dissolved in cold water and sodium CMC is dissolved in hot
water. More particularly, 215.65 grams of Klucel HFF are add to 4
liters of distilled water at room temperature and mixed in a Hobart
mixer for 2 hours. Concurrently, 11.35 grams of sodium CMC, type
7H3SF, are slowly added to 900 ml of distilled water at 70.degree.
C. while stirring and mixed for 2 hours. Then the sodium CMC
solution is slowly added to the HPC solution in the Hobart mixer
while mixing at slow speed and mixed for an additional 4 hours.
Although the specific example provided herein employs 11.35 grams
sodium CMC:215.56 grams HPC, it is understood that given the
teachings of the present invention, one of skill in the art will be
able to use more or less sodium CMC and/or HPC to arrive at a
matrix composition that will be useful as described herein.
[0042] Once the sodium CMC solution has been uniformly incorporated
into the HPC solution, the mixture is removed from the Hobart
mixer, spread onto Teflon coated trays and placed in a forced air
oven to be dried at a temperature of between about 20.degree. C.
and about 40.degree. C. In particularly preferred embodiments, the
drying temperature is 32.degree. C. These layers are allowed to dry
for approximately 6 hours, peeled off, turned over and allowed to
dry at modest temperatures for a further 24 hours. This drying
process removes any excess water. The inventors have discovered
that for curing to occur properly, it is important to remove this
excess water. Further, if this water is not removed at a low drying
temperature, a phase separation occurs between the sodium CMC and
HPC thereby resulting in a loss of integrity of the matrix.
[0043] Once the CMC/HPC layers have been dried they are cured at an
appropriate temperature and time in a vacuum oven. For example, the
layers are cured for between about 4 to about 48 hours at
temperatures of between about 120.degree. C. to about 250.degree.
C. Particular embodiments envision curing the layers for 24 hours
at between about 125.degree. C. to about 140.degree. C. Of course
it is understood that this is an exemplary temperature range and
any temperature between these two temperatures or any other
temperature conventionally used to cure polymeric materials will be
useful in this context of the invention. Thus it is understood that
any such temperature may be employed so long as the integrity of
the HPC/CMC matrix is maintained. As an alternative to drying in a
vacuum oven, the matrix may be cured in a conventional oven using
somewhat higher temperatures. For example, the matrix may be cured
at between about 140.degree. C. and about 200.degree. C. for 6-8
hours in a conventional oven. Again it is understood that these are
merely exemplary conditions and one of skill in the art may cure
the matrix at temperatures higher or lower than the 140.degree. C.
to 200.degree. C. temperature in a conventional oven for a suitable
period of time that the matrix is appropriately cured. One test for
ensuring that the matrix is appropriately cured is to employ the
wet finger test as described herein above. Once the matrix has been
cured it can be ground into a powder, have flavor incorporated
therein and added to the gum formulation. Preferably, the matrix is
ground to a size wherein it will pass through a 20 mesh sieve.
[0044] While not being bound by any particular theory, the
inventors suggest that the above mixing, drying and curing
procedures may result in some type of bonding, which might give the
properties of a cross-linked HPC matrix. It is also possible that
this process gives a self cross-linked product, or that at the
conditions given above, radicals may form within HPC, which may
bound within the HPC molecule. Hydrogen bonding may also modify the
physical properties of the cellulosic materials to give the desired
properties. Another theory is that a mixed crystalline/amorphous
matrix of HPC may form to give a lower solubility.
[0045] The HPC material may be dissolved in water, dried and cured
under similar conditions as above without the presence of any other
cross-linking agents to yield a matrix that may also act as a
flavor absorbent core. The curing process that gives the HPC/CMC
matrix its desirable properties may also give the cured HPC matrix
similar properties such as lower water solubility, and the HPC
matrix may similarly pass the wet finger test. Flavors may then be
absorbed onto the cores at levels as high as 40-60% and the
flavor/core matrix can then be added to a chewing formulation to
obtain longer lasting flavor.
[0046] If molecular blending was not necessary between HPC and CMC
or with HPC by itself, it may be possible that less water may be
needed to obtain a cured HPC with the desired properties. The
advantage would be that less drying would be needed which could
significantly reduce processing time. The amount of water to be
used may be as low as 1 part water to 9 parts HPC or even as low as
1 part water to 19 parts HPC. Sufficient water should be provided
to mobilize the HPC molecules such that the HPC molecules have more
of a chance to recombine with neighboring molecules to alter the
physical structure and solubility of HPC. However, it should be
noted that drying and curing HPC by itself without a sufficient
amount of water is not expected to have a significant effect.
[0047] Manufacture of Chewing Gum
[0048] The long flavor duration release structures of the present
invention can be used in typical chewing gum compositions. In
general, a chewing gum composition typically comprises a water
soluble bulk portion added to the water insoluble chewable gum base
portion. The flavoring agents are typically water insoluble. The
water soluble portion dissipates with a portion of the flavoring
agent over a period of time during chewing, while the bum base
portion is retained in the mouth throughout the chew.
[0049] The water soluble portion of the chewing gum may further
comprise softeners, sweeteners, flavoring agents and combinations
thereof. Softeners are added to the chewing gum in order to
optimize the chewability and mouth feel of the gum. Softeners, also
known in the art as plasticizers or plasticizing agents, generally
constitute between about 0.5 to about 15.0 percent by weight of the
chewing gum. Softeners contemplated by the present invention
include glycerin, lecithin, and combinations thereof. Further,
aqueous sweetener solutions such as those containing sorbitol,
hydrogenated starch hydrolysates, corn syrup and combinations
thereof may be used as softeners and binding agents in the chewing
gum.
[0050] Sugar sweeteners generally include saccharide containing
components commonly known in the chewing gum art which comprise but
are not limited to sucrose, dextrose, maltose, dextrin, dried
invert sugar, fructose, levulose, galactose, corn syrup solids, and
the like, alone or in any combination. Non-sugar sweeteners can
include sorbitol, mannitol, and xylitol.
[0051] Optional ingredients such as colors, emulsifiers and
pharmaceutical agents may be added to the chewing gum.
[0052] In general, chewing gum is manufactured by sequentially
adding the various chewing gum ingredients to a commercially
available mixer known in the art. After the ingredients have been
thoroughly mixed, the gum mass is discharged from the mixer and
shaped into the desired form such as by rolling into sheets and
cutting into sticks, extruding into chunks or casting into
pellets.
[0053] Generally, the ingredients are mixed by first melting the
gum base and adding it to the running mixer. The base may also be
melted in the mixer itself. Color or emulsifiers may also be added
at this time. A softener such as glycerin may also be added at this
time along with syrup and a portion of bulking agent. Further
portions of the bulking agent is typically added with the final
portion of the bulking agent.
[0054] The entire mixing procedure typically takes about fifteen
minutes, but longer mixing times may sometimes be required. Those
skilled in the art will recognize that many variations of the
above-described procedure may be followed.
[0055] The flavoring agent can be added after formation of the
matrix and grinding to form flavor cores of a desirable size by
soaking the cores in a beaker of flavoring agent. Another method of
adding flavoring agent is by misting the flavoring agent over the
cores. Although these methods will work, it is preferred to obtain
as homogeneous a distribution of the flavoring agent in the cores
as is possible. One such way to obtain a homogeneous distribution
is by using a Vee mixer. The Vee mixer has nozzles that mists the
flavoring agent over the cores as they are tumbled. Vee mixers can
be obtained from Patterson Industries (Canada) Limited. A Cone
Shell Blender is another type of mixer that will achieve the
desired uniform distribution of flavoring agent in the core.
Although in most cases the flavoring agent will be absorbed into
the cores very rapidly, it is desirable to allow the cores to mix
for a sufficient time to reach equilibrium.
[0056] The flavoring agent is releasably retained by the cores, to
the extent that it is released when gum containing the flavor
releasing structures is chewed. Additionally, different and
multiple flavoring agents may be used in a single core. The cores
can contain very large amounts of flavoring agent. For example,
cores have been made that contained as much as 40 to 60% flavoring
agent based on the total weight of the core. Although 33% loading,
based on the total weight of the core is presently preferred. The
higher the loading the faster the flavoring agent will be released
from the core, all other factors being equal.
[0057] Flavorings And Other Gum Components
[0058] Flavoring agents may comprise essential oils, synthetic
flavors, or mixture thereof including but not limited to oils
derived from plants and fruits such as citrus oils, fruit essences,
peppermint oil, spearmint oil, clove oil, oil of wintergreen,
anise, and the like. Artificial flavoring agents are also
contemplated. Those skilled in the art will recognize that natural
and artificial flavoring agents may be combined in any sensorially
acceptable blend. All such flavors and flavor blends are
contemplated by the present invention, including by way of example,
peppermint, spearmint, wintergreen, cinnamon, menthol, eucalyptus,
and other fruit and citrus flavorings. Besides the flavored cores,
additional flavor may be added to the chewing gum composition by
conventional means.
[0059] Once the flavoring agent is retained in the core, the core
can optimally be coated with a flavor barrier coating. The coating
increases the shelf life of the flavor releasing structure when it
is incorporated into a chewing gum. The coating also aids in
handling and processing the cores by preventing the flavor from
evaporating. The coating can prevent the flavor from migrating into
the gum and can protect chemically sensitive flavoring agents from
reacting with the ingredients of the gum. The coating can also
affect the release rate of the flavoring agent. Generally, any
natural or synthetic material that exhibits a flavor barrier
characteristic can be used for the coating.
[0060] Once the flavor releasing structure has been formed, it is
then incorporated into a chewing gum. Addition to the gum mixer
during the last stage of the mixing cycle is preferred to minimize
any damage to the flavor releasing structures.
[0061] Chewing gum consists of a gum base to which a water soluble
bulk portion may normally be added. Chewing gum bases generally
comprise a combination of elastomers and resins together with
plasticizers and inorganic fillers.
[0062] The gum base may contain natural gums and/or synthetic
elastomers and resins. Natural gums include both elastomers and
resins. Suitable natural gums include, but are not limited to
chicle, jellutong, sorva, nispero tunu, niger gutta, massaranduba
belata, and chiquibul.
[0063] When no natural gums are used, the gum base is referred to
as "synthetic" and the natural gums are replaced with synthetic
elastomers and resins. Synthetic elastomers may include
polyisoprene, polyisobutylene, isobutylene-isoprene copolymer,
styrene butadiene rubber, a copolymer form Exxon Corp. under the
designation "butyl rubber," and the like.
[0064] The amount of elastomer used in the gum base can typically
be varied between about 10 and about 20 percent depending on the
specific elastomer selected and on the physical properties desired
in the final gum base. For example, the viscosity, softening point,
and elasticity can be varied.
[0065] Resins used in gum bases may include polyvinylacetate,
polyethylene, ester gums, (resin esters of glycerol),
polyvinylacetate polyethylene copolymers, polyvinylacetate
polyvinyl laureate copolymers, and polyterpenes. As with the
elastomer, the amount of resin used in the gum base can be varied
depending on the particular resin selected and on the physical
properties desired in the final gum base.
[0066] Preferably, the gum base also includes plasticizers selected
from the group consisting of fats, oils, waxes, and mixtures
thereof. The fats and oils can include tallow, hydrogenated and
partially hydrogenated vegetable oils, and cocoa butter. Commonly
employed waxes include paraffin, microcrystalline and natural waxes
such as beeswax and carnauba. Additionally, mixtures of the
plasticizers may be used such as a mixture of paraffin wax,
partially hydrogenated vegetable oil, and glycerol
monostearate.
[0067] Preferably, the gum base also includes a filler component.
The filler component is preferably selected from the group
consisting of calcium carbonate, magnesium carbonate, talc,
dicalcium phosphate and the like. The filler may constitute between
about 5 to about 60 percent by weight of the gum base. Preferably,
the filler comprises about 5 to about 50 percent by weight of the
gum base.
[0068] Further, gum bases may also contain optional ingredients
such as antioxidants, colors, and emulsifiers.
[0069] These ingredients of the gum base can be combined in a
conventional manner. In particular, the elastomer, resins,
plasticizers, and the filler are typically softened by heating and
then mixed for a time sufficient to insure a homogenous mass. The
mass can be formed into slabs, or pellets and allowed to cool
before use in making chewing gum. Alternatively, the molten mass
can be used directly in a chewing gum making process.
[0070] Typically, the gum base constitutes between about 5 to about
95 percent by weight of the gum. More preferably the insoluble gum
base comprises between 10 and 50 percent by weight of the gum and
most preferably about 20 to about 35 percent by weight of the
gum.
EXAMPLES
[0071] The following examples are included to demonstrate preferred
embodiments of the invention. It should be appreciated by those of
skill in the art that the techniques disclosed in the examples
which follow represent techniques discovered by the inventors to
function well in the practice of the invention, and thus can be
considered to constitute preferred modes for its practice. However,
those of skill in the art should, in light of the present
disclosure, appreciate that many changes can be made in the
specific embodiments which are disclosed and still obtain a like or
similar result without departing from the spirit and scope of the
invention.
[0072] The following protocol provides an exemplary methods for
making the HPC/CMC matrices of the present invention. Of course it
is understood that this is merely an exemplary protocol and that
one of skill in the art will readily be able to adapt the weights,
temperatures and times used in the procedure and still arrive at a
matrix that will be useful in the present invention.
[0073] 1. Weigh 215.65 grams of Klucel HFF (high MW HPC) and add to
4 liters of distilled water at room temperature and mix in a Hobart
mixer for 2 hours.
[0074] 2. Weigh 11.35 grams of sodium carboxylmethylcellulose
(sodium CMC), type 7H3SF, and slowly add to 900 ml of distilled
water at 70.degree. C. while stirring and mix for 2 hours.
[0075] 3. Add sodium CMC solution slowly to HPC solution in the
Hobart mixer while mixing at slow speed and mix for an additional 4
hours.
[0076] 4. Remove HPC/CMC mix from Hobart and spread on Teflon
coated trays and place materials in forced air oven at 90.degree.
F.
[0077] 5. Allow to dry for 6 hours, peel off partially dried
mixture and turn over and dry 24 hours.
[0078] 6. This material is then dried and cured for 24 hours at 125
to 140.degree. C. in a vacuum oven and ground.
[0079] The inventors believe that this process facilitates a
cross-linking between HPC and sodium CMC. However, it may be that
this process gives a self cross-linked product, or that at the
conditions given above, radicals may form within HPC, which may
bound within the HPC molecule.
[0080] In order to determine if the HPC and sodium CMC polymers are
properly cured a preliminary test may be performed. When wetted on
the fingers, the polymers will appear to dissolve and give a wet,
slimy feel. If the polymers are properly cured, they will not
dissolve in water, nor will a slimy film form on the fingers. These
cured polymers will be solid and can be ground. This will allow
this matrix to swell and adsorb flavors for use in gum. The process
of the present invention yields a solid matrix that has a very low
water solubility. Preferably, such a very low water solubility
would be even lower than the water solubility of high MW HPC.
[0081] When the flavor is absorbed onto the matrix material,
non-sticky solid particles are formed that swell in size. If too
much sodium CMC is used, the cross-link density may be too high and
not as much flavor may be absorbed. A low cross-link density is
desired, so a low level of sodium CMC should be used, preferably
less than about 10% of the HPC material and more preferably less
than about 5% of the HPC material.
[0082] The flavor, such as a peppermint flavor blend, is mixed with
the HPC/CMC matrix and allowed to set 3-4 hours. The particles
remain as solid particles, but when swelled are soft particles, and
can be added directly to a chewing gum formulation. In example 2
below, two parts of the HPC/CMC matrix with 5% sodium CMC was made
and ground to less than 20-mesh, used as cores, and mixed with one
part peppermint flavor and allowed to set for 4 hours. As a
comparison, a HPC/silica/glycerol monostearate matrix in
comparative Example 1 was made at a 60/20/20 ratio and mixed with
peppermint flavor at a 2/1 ratio of core/flavor as described in PCT
Patent Publication No. WO 94-14330 and used for comparison
purposes. The following gum formula was used to make Examples 1
and2.
1 COMPONENT PERCENTAGE CONTENT Base 18.75 Sugar 51.52 39 DE, 45.5
Be Syrup 12.71 Dextrose Monohydrate 9.45 Glycerin 1.23 Peppermint
Flavor 0.86 Encapsulated Sweeteners 3.26 Lecithin 0.24 Polymer
Core/Flavor Matrix 1.98 TOTAL % 100.00
[0083] Examples 1 and 2 were compared in a blind test for flavor
intensity by a 9 member panel and data are shown in the FIG. 1.
Results show that the HPC/CMC matrix gave an improved flavor
intensity throughout most of the chewing period compared to the
previously made flavored cores. The comparison sample had
previously shown an improved flavor release compared to standard
products, which indicates the new HPC/CMC flavored matrix gives an
even more improved flavor release. Also, when used at the level of
about 2% HPC in the chewing gum composition, the flavor cores of
comparative Example 1 produced a slimy texture. However, the use of
2% of HPC in the gum of Example 2 did not produce a slimy
texture.
[0084] All of the compositions and/or methods disclosed and claimed
herein can be made and executed without undue experimentation in
light of the present disclosure. While the compositions and methods
of this invention have been described in terms of preferred
embodiments, it will be apparent to those of skill in the art that
variations may be applied to the compositions and/or methods and in
the steps or in the sequence of steps of the method described
herein without departing from the concept, spirit and scope of the
invention. More specifically, it will be apparent that certain
agents which are both chemically and physiologically related may be
substituted for the agents described herein while the same or
similar results would be achieved. All such similar substitutes and
modifications apparent to those skilled in the art are deemed to be
within the spirit, scope and concept of the invention as defined by
the appended claims.
* * * * *