U.S. patent application number 15/407384 was filed with the patent office on 2017-05-04 for xylitol containing comestible product.
The applicant listed for this patent is The Hershey Company. Invention is credited to Ashley L. Boldt, Burton Douglas Brown, Thomas J. Carroll, Paula M. Gibson, Robert J. Huzinec, Steven M. Kumiega, David M. Stumpf.
Application Number | 20170119797 15/407384 |
Document ID | / |
Family ID | 43628685 |
Filed Date | 2017-05-04 |
United States Patent
Application |
20170119797 |
Kind Code |
A1 |
Kumiega; Steven M. ; et
al. |
May 4, 2017 |
XYLITOL CONTAINING COMESTIBLE PRODUCT
Abstract
The present invention relates to a process for preparing a
comestible product comprising xylitol said method comprising: (a)
subjecting a composition comprising xylitol in an amount ranging
from about 60% to about 100% by weight to extrusion treatment
inside an extrusion apparatus under conditions sufficient to form
and maintain the xylitol in a slurry and (b) then shaping the
extruded slurry and cooling the product to form a solid. The
present invention additionally is directed to a product produced
therefrom.
Inventors: |
Kumiega; Steven M.;
(Hummelstown, PA) ; Carroll; Thomas J.;
(Mechanicsburg, PA) ; Boldt; Ashley L.;
(Harrisburg, PA) ; Gibson; Paula M.; (Harrisburg,
PA) ; Huzinec; Robert J.; (Hummelstown, PA) ;
Brown; Burton Douglas; (Hershey, PA) ; Stumpf; David
M.; (Palmyra, PA) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
The Hershey Company |
Hershey |
PA |
US |
|
|
Family ID: |
43628685 |
Appl. No.: |
15/407384 |
Filed: |
January 17, 2017 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
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14868471 |
Sep 29, 2015 |
9572772 |
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15407384 |
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13392689 |
Feb 27, 2012 |
9179695 |
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PCT/US10/47071 |
Aug 30, 2010 |
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14868471 |
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61238017 |
Aug 28, 2009 |
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Current U.S.
Class: |
1/1 |
Current CPC
Class: |
A61K 9/145 20130101;
A61K 47/18 20130101; B29C 48/04 20190201; A23G 3/0021 20130101;
A23G 3/42 20130101; A61K 31/616 20130101; A23P 10/25 20160801; A61K
47/26 20130101; A23P 30/20 20160801; A23L 27/34 20160801; A23G 3/38
20130101; A61P 25/04 20180101; A61P 29/00 20180101; A23L 29/37
20160801; A61K 9/0056 20130101; A61K 47/10 20130101; A23V 2002/00
20130101 |
International
Class: |
A61K 31/616 20060101
A61K031/616; A23L 29/30 20060101 A23L029/30; A61K 9/14 20060101
A61K009/14; A23L 27/30 20060101 A23L027/30; A61K 9/00 20060101
A61K009/00; A61K 47/26 20060101 A61K047/26 |
Claims
1.-27. (canceled)
28. A solid homogenous non-compressible comestible product
comprising from about 60% up to and including 100% solid xylitol,
by weight and substantially free of any other sugar alcohol and
substantially free of monosacchrides and dissachrides and
maltodextrin having a DE of less than 20, and having a moisture
content of less than about 1% by weight, said product, if formed
into a yertz shape and having a base width of 8.20 mm and a length
of about 13.26 mm, a height of 8.71 mm, a 10% angle between the
vertical and a side thereof and having 0.25 mm fillet and weighing
about 0.75 grams, exhibits a piece break pressure of less than
about 110 MPa and a dissolution rate in water from about 200 to
about 400 seconds.
29. The comestible product according to claim 28 comprised of at
least about 70% by weight xylitol.
30. The comestible product according to claim 29 comprised of at
least about 80% by weight xylitol.
31. The comestible product according to claim 30 comprised of at
least about 95% by weight xylitol.
32. The comestible product according to claim 28 comprising one or
more additional ingredients selected from the flavorants, coloring
agents, cooling agents, food additives and food grade processing
agents.
33. The comestible product according to claim 28 wherein sodium
bicarbonate is additionally present.
34. The comestible product according to claim 31 wherein sodium
bicarbonate is present.
35. The comestible product according to claim 28 additionally
comprising a pharmaceutical.
36. The comestible product according to claim 35 wherein the
pharmaceutical is an analgesic.
37. The comestible product according to claim 36 wherein the
analgesic is aspmn.
38. The comestible product according to claim 35 wherein the
pharmaceutical is present in therapeutically effective amounts and
up to about 40% by weight.
39. The comestible product according to claim 38 where the
pharmaceutical is present in amounts ranging from about 0.01% to
about 40% by weight.
40. The comestible product according to claim 28 in the form of a
disc.
Description
FIELD OF THE INVENTION
[0001] The present invention relates to a process for the
production of a non-compressible comestible product comprising
xylitol and the comestible product comprising xylitol produced
therefrom.
BACKGROUND OF THE INVENTION
[0002] Xylitol is a naturally occurring five carbon sugar alcohol.
It occurs naturally in many fruits and vegetables and is produced
by the human body during normal metabolism. It is a sweet
crystalline product, white in color, odorless and soluble in water.
In crystalline form, it quickly dissolves in the mouth. It has a
negative heat of dissolution, and thereby produces an agreeable
refreshing or cooling effect in the mouth.
[0003] In addition to its cooling effect, xylitol has interesting
sweetening qualities. If one takes sucrose as a reference point,
and attributes to it a sweetening value of 1, xylitol is found to
have a sweetness of the same order. Thus, xylitol is a sugar
substitute. In fact, it has the same sweetness and bulk as sucrose
with one third fewer calories (2.4 calories per gram) and no
unpleasant after taste. It is currently approved around the world
for use in foods, pharmaceuticals and oral hygiene products. For
example, xylitol has been widely used in confectionery, baking
products, cereals, desserts, jams, beverages, chocolate, chewing
guru, gumdrops, and ice cream to name just a few products. It has
also been used in the production of oral hygiene products, such as
toothpaste and in pharmaceutical products. In addition, it is used
as a sucrose substitute placed in foods for consumption by people
with diabetes.
[0004] Further, xylitol has an interesting property for dental
health, in which it differs from other known polyols. It is, in
fact, anti-cariogenic, i.e., it cannot serve as a substrate for
bacteria present in the mouth cavity. Moreover, it also plays a
role in preventing dental caries. It inhibits the growth of
Streptococcus Mutans, the primary bacteria associated with dental
caries. Recent interest has increased in xylitol-containing candies
because xylitol has been shown to promote remineralization of teeth
and damaged tooth enamel. It has also been found that regular use
of xylitol can inhibit the transfer of cariogenic Streptococcus
Mutans bacteria from mothers to their newborn children. Studies
have shown that mothers are the primary source of infection of
Streptococcus in the mouths of newborns and that prevention or
delaying colonization by these bacteria leads to significant
reduction in tooth decay later in life. In addition, xylitol
reduces plaque accumulation and inhibits plaque regrowth.
[0005] Further, it also increases salivary flow. Saliva helps clean
and protect teeth from decay and this plays a role in repairing the
damage caused in the early state of the decay process.
[0006] Thus, it is important to have a method of producing products
comprising xylitol for use in these various applications. One such
product is a hard candy comprised of xylitol. However, producing a
hard candy of xylitol is challenging. It is difficult for xylitol
to be made into a hard candy free of crystals because its glass
transition is below 32 F.(0 C.) and at normal household conditions,
it would exist as a liquid, although because of its instability,
would slowly transform to a few large crystals grown loosely
together. Furthermore, as a crystal, it does not compact well.
[0007] In addition, in preparing hard candies comprising xylitol,
the xylitol is traditionally melted completely to form a molten
mass. The molten mass is mechanically agitated or seeded with
xylitol crystals to cause crystallization. The resultant seeded
mass is then combined in a layered format, wherein an isomalt base
is first deposited, then followed by a xylitol layer or the xylitol
is codeposited with isomalt in a mold to produce hard candy.
[0008] The problem often encountered in this process is that the
final product is usually hygroscopic and sticky. Further, the
molten mass often manages to crystallize in the machinery and/or
equipment, thereby clogging the machinery and/or equipment.
Further, once the seed crystals have been added, the viscosity of
the seeded molten mass is very difficult to control. Moreover, the
product is very temperature sensitive. The seeded mass thickens and
crystallizes rapidly if the temperature falls below the melting
point of xylitol, and on the other hand, thins, due to melting of
the seed crystals if the temperature is raised above the melting
point. As a consequence, the viscosity and density of the seeded
mass tends to vary upon prolonged exposure to a molten state which
is particularly undesirable in deposited hard candy manufacturing
lines where an inconsistency of the seeded mass leads to
inconsistent piece weight and potential equipment failure. Further,
the resultant candy is quite hard, and difficult to bite
through.
[0009] The present inventors were investigating a new method for
producing a hard candy comprising xylitol by modifying the
methodology of the prior art. They began preparing the hard candy
in a scraped surface heat exchanger, maintaining the temperature at
or above the melting point of xylitol. Even though they initially
worked with a complete melt, when they lowered the temperature in
the scraped surface heat exchanger below the melting point of
xylitol, crystals of xylitol began to form in the scraped surface
heat exchanger and begin to clog the machine. Once the xylitol
recrystallized, it became extremely difficult to work with. The
inventors also noted that the product was hard and was not easily
bitten into. Moreover, the inventors have confirmed that if the
temperature of the emitted scraped surface heat exchanger was too
hot, such material was difficult to handle and the product obtained
was undesirable.
[0010] However, the inventors found that if the xylitol was not
completely melted in an extruder, the resulting product was
different and was much softer than the product comprising xylitol
obtained from completely melting the solid and recystallizing the
melted solid in a scraped surface heat exchanger. Further, in the
method found by the present inventors, since the xylitol solid was
not being recrystallized, the extruder was no longer getting
clogged.
[0011] The present invention thus describes this process which
overcomes the problems enumerated above and provides a product
which has a high flavor impact and a strong cooling sensation. Yet,
at the same time, the product that is produced is a soft product
that can be easily bitten through.
SUMMARY OF THE INVENTION
[0012] The present invention, in one embodiment, is directed to a
method of producing a solid non-compressible comestible product
comprising xylitol, said method comprising: [0013] (a) subjecting a
composition comprising solid xylitol in an amount ranging from
about 60% up to and including 100% by weight to extrusion treatment
in an extrusion apparatus under conditions sufficient to partially
melt the xylitol in the composition to form a slurry and maintain
the composition as a slurry as it passes through and exits the
extrusion apparatus, [0014] (b) forming the extruded product from
step (a) into a desired shape and [0015] (c) cooling the product of
(b) to form a solid.
[0016] The present invention is also directed to the product of the
process described hereinabove. In an embodiment, it is a comestible
comprising from about 60% to about 100% xylitol, having irregularly
shaped crystals, and which, when molded into a yertz shape having a
base width of 8.20 mm, a base length of 13.26 mm, a height of 8.71
mm, an angle of 10% between the vertical and the side and having
0.25 mm radius fillet and weighing about 0.75 grams, has a piece
break pressure of less than about 110 MPa and a dissolution rate
from about 200 to about 400 seconds, said comestible having a
moisture content of less than about 1% by weight of the
composition, said comestible being substantially free of
monosaccharides and disaccharides and maltodextrin having a DE
(dextrose equivalent) of less than 20 and sugar alcohols other than
xylitol.
DESCRIPTION OF THE DRAWINGS
[0017] FIG. 1 illustrates a single screw extruder system that can
be utilized in the present invention.
[0018] FIGS. 2a, 2b and 2c each depict a cross section of the
extruder system in FIG. 1.
[0019] FIG. 3 is an embodiment of a depositor.
[0020] FIG. 4 is a microscopic image magnified 400.times. of a drop
of the xylitol composition in Example 10.
[0021] FIG. 5 is a photomicrograph of the drop deposited xylitol
composition from Example 11.
[0022] FIG. 6a-6c represent photographs of a xylitol composition
molded into a yertz shape. FIG. 6a is a front view, while FIG. 6b
is a top view and FIG. 6c is a side view.
DETAILED DESCRIPTION OF THE INVENTION
[0023] As described hereinabove, an embodiment of the present
invention is directed to a process of preparing a comestible
product comprised of xylitol. The comestible product within the
scope of the present invention includes hard candies, drops, such
as fruit drops or cough drops or candy drops, and the like or any
molded shaped product comprised substantially of xylitol.
Alternatively, the comestible product may be a pharmaceutical. The
product may be uncoated or coated with coatings normally used in
the confectionery arts. In an embodiment, the product, including
the coating, is substantially sugar free, e.g., contains no sugar,
such as sucrose. As used herein, the term "sugar" refers to aldoses
and ketoses, which are monosaccharides or disaccharides.
[0024] These sugars which are excluded include, without limit,
erythrose, threose, ribose, arabinose, xylose, lyxose, allose,
altrose, glucose, mannose, gulose, idose, galactose, talose,
erythrulose, ribulose, xyulose, psicose, fructose, sorbose,
tagatose, maltose, lactose, sucrose and the like. By being
"substantially free", it is meant that the product contains at
most, if any, trace amounts of any sugar, i.e., the sugar content
is less than about 1% by weight.
[0025] The major ingredient of the comestible product of the
present invention is xylitol. Xylitol is commercially available in
a crystalline form (or granulated form). Either form of xylitol may
be used in the comestible product of the present invention.
[0026] The comestible product contains at least about 60% by weigh
xylitol. In one embodiment, the comestible product contains from
about 60% xylitol up to and including 100% xylitol by weight and in
another embodiment, from about 70% xylitol up to and including 100%
xylitol by weight and in a still another embodiment from about 80%
up to including 100% xylitol by weight. In another embodiment, the
comestible product contains from about 85% xylitol to 100% xylitol
by weight and in a still further embodiment, the comestible product
contains from about 90% xylitol up to and including 100% xylitol by
weight. In a still further embodiment, the comestible product
contains from about 95% xylitol up to and including 100% xylitol by
weight. Thus, in one embodiment, the comestible product contains
solely xylitol.
[0027] In one embodiment, the xylitol is in association with
another active product, e.g., a pharmaceutical. In an embodiment,
the composition contains as much drug as possible, for example, up
to and about 40% by weight drug. In an embodiment the composition
comprises from about 0.01% to about 40% by weight drug, and at
least about 60% xylitol by weight such as, for example, from about
60% to about 99.99% xylitol by weight
[0028] When xylitol is the sole active ingredient or when the
comestible product is a hard candy, drop or molded product, the
objective is to maximize the concentration of xylitol. In an
embodiment, the xylitol is present in at least from about 70% by
weight to about 100% by weight and in another embodiment, the
xylitol is present in amount varying from about 80% to about 100%
by weight.
[0029] Besides xylitol, the comestible product optionally contains
flavorants, such as one or more food grade acids that are
conventionally used in confectionery products. In an embodiment,
these flavorants are present in flavoring effective amounts. An
example of a flavorant is food grade acid. In one embodiment, the
one or more food grade acids are present in amounts ranging from
about 0.01% to about 10% by weight of the product. In another
embodiment, they are present in an amount ranging from about 0.01%
to about 5% of the product, and in still another embodiment from
about 2% to about 4% by weight of the product.
[0030] Examples of food grade acids that may be used in the present
invention include, but are not limited to, malic acid, lactic acid,
acetic acid, citric acid, fumaric acid, adipic acid, tartaric acid,
ascorbic acid, phosphoric or salts of any of the food grade acids.
The comestible composition thus may comprise xylitol and optionally
one food grade acid or salt thereof or a combination of one or more
food grade acids or salts thereof.
[0031] The comestible composition may optionally contain other
ingredients normally found in confections. For example, the
composition may additionally contain other compounds, such as
vitamins, minerals or other dietary substances that have the proper
stability, i.e. they are stable under the conditions for forming
the comestible composition of the present invention. In addition,
the composition may also contain other flavoring agents in addition
to or in lieu of the food grade acids.
[0032] The other flavors useful in the present invention are
flavors well known for use in comestible products, such as foods,
e.g., confections. The flavorant may no in solid form, such as a
powder, crystalline, amorphous crystal, semicrystalline and the
like. They may be in the form of liquids or they may be
encapsulated or they may be spray dried. The additional flavors
include those derived from essential oils, as well as those flavors
characterized as either natural or artificial flavors. Examples
include essential oils such as, without limitation, cinnamon,
spearmint, peppermint, birch, and the like; natural or artificial
fruit flavors, such as, without limitation, apple, pear, peach,
strawberry, cherry, apricot, orange, lemon, watermelon, banana, and
the like; bean derived flavors such as, without limitation, coffee,
cocoa powder and the like. In another embodiment, the flavoring
agent may be a spice commonly used in foods. Examples include chili
powder, curry powder and the like in another embodiment, the
flavorant may be a salt commonly used in the food arts, such as
sodium chloride, potassium iodide, potassium chloride, sodium
iodide and the like. In another embodiment, the comestible product
of the present invention contains one or more flavorants.
[0033] However, those flavors derived from the essence of mint oils
are preferred. In the instance where flavors, such as peppermint,
spearmint and the like are prepared in accordance with the present
invention, the resulting flavor composite yields a particularly
cooling taste sensation. The cooling effect is attributable to the
presence of xylitol in the solid crystalline form in combination
with the mint oil. Thus, flavor enhancement is a further feature
and benefit of the present invention.
[0034] As with the food grade acids, these flavoring agents are
present in flavoring effective amounts. For example, they are
present in amounts ranging from about 0.01% to about 10% by weight
and in another amount from about 0.01% to about 5% by weight of the
composition.
[0035] In addition, another optional ingredient is a cooling agent,
i.e., an ingredient that imparts a cooling perception to the
consumer when ingested. Examples include such agents as menthol,
lemon aromas, WS 23, which is
N,2,3-trimethyl-2-(1-methyl-ethyl)-butanamide, and the like. Even
without the additional coolant, the comestible xylitol product
dissolves quickly in the mouth and the coolness effect of the
xylitol is felt by the consumer quite quickly. The additional
coolant, if present, enhances the coolness effect felt by the
consumer. In an embodiment, the cooling agent is present in an
amount from about 0.01% to about 2% by weight of the composition
and in another embodiment from about 0.05% to about 1% by weight if
the comestible product.
[0036] However, some sugar alcohols are cooling agents.
Nevertheless, the comestible product is substantially free of sugar
alcohols other than xylitol. By substantially free, it is meant
that if the comestible product contains a sugar alcohol other than
xylitol, then the sugar alcohol is present in such low
concentrations that it does not affect any of the properties
described herein, such as the dissolution rate, the break pressure
point, and the like. In one embodiment, the comestible product
contains no sugar alcohol and in another embodiment, it contains
trace amounts of sugar alcohol, for example, less than about 2.0%
by weight of sugar alcohol, and in another embodiment, the sugar
alcohol is present in less than about 1.0% by weight of the
product. The cooling agents are those commercially available
cooling agents normally used in the confectionery arts, except for
the sugar alcohols other than xylitol, provided these other sugar
alcohols are present in trace amounts, as described herein.
[0037] In another embodiment, the composition of the present
invention is substantially free of sugars, such as monosaccharide,
disaccharide and polysaccharide.
[0038] Cooling agents, when present, are present in an amount
effective to enhance the coolness effect felt by consumers. In an
embodiment, they are present in an amount ranging from about 0.01%
to about 1% by weight of the product, and in another embodiment,
are present in an amounts ranging from 0.01% to about 0.5% by
weight of the comestible product.
[0039] There can also be added synthetic or natural food grade
coloring agents, such as, for example but not limited to, azo
coloring agents or carotenoids (e.g., B carotene, canthaxathin and
the like), and the like.
[0040] The total amount of these coloring agents should not exceed
about 5% wt of the composition. They may be present in as low as
0.001% by weight of the product.
[0041] In addition, sodium bicarbonate can also be present. Its
presence effects dissolution and provides a unique texture to the
composition. In an embodiment, when present, sodium bicarbonate
reduces the density of the mixture. In an embodiment, the sodium
bicarbonate is present in an amount effective to reduce the density
of the composition relative to the density before addition thereof.
In an embodiment, sodium bicarbonate is present in an amount
ranging from about 0.01% to about 10%, and in another embodiment
from about 0.01% to about 5% by weight, and in another embodiment
from about 0.01% to about 3% by weight of the comestible
product.
[0042] Other additional components that can be present in the
comestible product of the present invention include one or more
food grade processing agents and food additives which are typically
used in confectionery products. Examples include, but are not
limited to, food grade preservatives, and the like. If present,
they are present in amounts ranging from about 0.01% to about 5% by
weight of the product.
[0043] These optional additives described hereinabove, such as food
additives, e.g., food-grade acids, flavoring agents, coloring
agents, food grade preservatives, and any other components that are
typically used in confectionery products may be added as solids, or
liquid form or may be pre-dried. The total amount of these optional
ingredients, however, does not exceed about 40% by weight of the
comestible product. In another embodiment, the total amount is no
more than about 30% by weight and in another embodiment, no more
than about 20% by weight, and in a still further embodiment no more
than about 10% by weight of the comestible product and in another
embodiment, no more than about 5% by weight of the comestible
product.
[0044] Besides candy, the comestible product may be a
pharmaceutical and may contain excipients known in the
pharmaceutical arts. The pharmaceutical may be present in solid
form, e.g., crystalline, semicrystalline or amorphous solid. The
pharmaceutical may be a liquid. In addition, the xylitol in the
comestible product may be present in combination with a
pharmaceutical such as pain-killers, e.g., aspirin, as described
herein. The pharmaceutical is present in a pharmaceutically
effective amount. The amount can be as low as 0.01% or 0.05% by
weight and up to and including about 40% by weight. The
pharmaceutical is present in a pharmaceutically effective amount.
For example, if the pharmaceutical is an analgesic, e.g., aspirin,
the analgesic is present in an analgesic effective amount. In an
embodiment, the pharmaceutical is present in an amount ranging from
about 0.1 to about 40% by weight. In another embodiment, it is
present in an amount of about 5 to about 35% by weight. In another
embodiment, the pharmaceutical is present in an amount ranging from
about 8% to about 32% by weight. As described hereinbelow, any
pharmaceutical can be utilized as long as the pharmaceutical does
not decompose under conditions, e.g., temperature conditions,
described herein in making the comestible product of the present
invention. When a pharmaceutical is present the xylitol may be
present from about 60% to about 99.9% by weight. In another
embodiment, the xylitol may be present in at least 90% by weight
and in another embodiment in at least 80%, by weight.
[0045] The comestible product of the present invention formed by
the present process has a very low moisture content. In an
embodiment, water is present in less than about 1% by weight of the
comestible product. In another embodiment, it is present in less
than about 0.5% by weight and in another embodiment, is present in
less than about 0.25% by weight.
[0046] An embodiment of the present invention is a comestible
product comprising from about 90% to about 99.9% by weight of
xylitol; and optionally from about 0.1% to about 5% by weight of
one or more food grade acids. In another embodiment, the comestible
product comprises from about 95% to about 99.9% by weight of
xylitol; and in another embodiment, the comestible product
comprises xylitol in about 95% to about 98% by weight and
optionally from about 2% to about 4% by weight of one or more food
grade acids.
[0047] In still another embodiment, besides the xylitol and
optionally the food grade acid the comestible product additionally
comprises a flavoring agent. In an embodiment, it additionally
comprises from about 0.01% to about 10% flavoring agent by weight.
In an embodiment, the comestible product comprises at least about
60% to about 100% by weight xylitol, optionally a flavoring agent,
optionally cooling agent or both optionally flavoring agent and
cooling agent. For example, in an embodiment the comestible product
comprises at least about 95% xylitol, about 0.1 to about 2%
flavoring agent and about 0.1 to about 0.5% cooling agent by
weight.
[0048] In a further embodiment, the comestible product comprises
xylitol and optionally one or more food grade acids, as described
hereinabove and optionally a food coloring agent and a cooling
agent. In a still another embodiment, the xylitol comestible
product comprises xylitol and optionally one or more food grade
acids in the amounts as described herein and about 0.001% to about
5% colorine agent.
[0049] In still another embodiment, the comestible product
comprises xylitol, optionally one or more food grade acids and a
coloring agent and a flavoring agent other than food grade acid and
a cooling agent, as described hereinabove.
[0050] In yet another embodiment, the comestible product of the
present invention comprises from about 90% to about 99.9% by weight
of xylitol, optionally from about 0.01% to about 5% by weight of
one or more food grade acids, and from about 0.01% to about 3% by
weight of sodium bicarbonate, A coloring agent may additionally be
present.
[0051] In an additional embodiment, the comestible product of the
present invention comprises from about 90% to about 99.9% by weight
of xylitol, optionally from about 0.01% to about 5% by weight of
one or more food grade acids, from about 0.01% to about 10% by
weight of one or more food grade flavoring agents, and from about
0.01% and about 3% by weight of sodium bicarbonate wherein the
total of the additives, e.g., flavoring agents, coloring agents and
sodium bicarbonate, does not exceed about 20% by weight of the
comestible composition.
[0052] In a still further embodiment, the comestible product of the
present invention comprises from about 60% to and including 100% by
weight of xylitol and optionally contains from about 0.01% to about
5% by weight of one or more food grade acids, and optionally up to
about 39.99% by weight of one or more food grade processing agents
and food additives.
[0053] It is to be understood, as used herein, that 100% xylitol
refers to the xylitol from a very substantially pure sample (e.g.,
having a xylitol concentration of greater than about 99.5% by
weight) being the sole component. It may contain trace amounts of
other components when manufactured, i.e., less than 0.5% by weight,
but the preparation of the comestible composition, in accordance
with the procedure hereinbelow does not add any additional
components.
[0054] The comestible product is prepared by utilizing techniques
known in the art, although the actual procedure was not known
heretofore. In the first step, the composition comprising xylitol
is placed into or fed into or passes through an extruder. If the
composition contains optional ingredients, i.e., ingredients other
than xylitol, a mixture comprising the xylitol and the other
ingredient is prepared by blending the xylitol solid and the
optional ingredients, e.g. cooling agent, flavoring agent, and the
like to form a substantially homogeneous mixture, i.e., all of the
ingredients are mixed thoroughly and are at least substantially
uniformly dispersed in the mixture. In another embodiment, the
various ingredients are uniformly mixed. The components are mixed
in an apparatus typically used in the art, for example, a mixer,
blender, shaker or static mixer and the like.
[0055] This mixing may be effected in a mixer separate from the
extruder, i.e., it may take place prior to the mixed composition
being placed into the extruder. In another embodiment, the mixing
takes place within the extruder. The extruder has regions, such as
a mixing zone, and the xylitol with any additional components
introduced into the mixing zone from a feed device, e.g., feed
hopper, pump and the like, is subjected to shearing force and
intense mechanical friction by the compression in the turns of the
screw. The blended xylitol composition enters the extrusion stream
and is subjected to the processes described hereinbelow.
[0056] This composition or if xylitol is the sole component,
xylitol (hereinafter, the composition being drawn through in the
extruder will be referred to as the "extruder composition") is
subjected to additional processing as described below. The extruder
optionally contains at least one extrusion die, although it is not
necessary. Inside the extruder, there are at least one or more
temperature zones which are set to predetermined temperatures. In
the present process, the temperature zones are set at temperature
to partially melt the xylitol so that in the extruder, the extruder
composition is only partially melted, that is, the xylitol is
molten and contains crystalline solid. By "partially melted", it is
meant that the mixture is not completely melted. In other words,
some solid material, xylitol, is maintained and not completely
melted, in accordance with the present process, seed crystals are
not necessary. In an embodiment of the present process, at least
about 10% by weight of the solid is melted, while in another
embodiment at least about 50% by weight of the solid is melted. In
a still further embodiment, at least about 90% of the solid is
melted. In a further embodiment, at least about 95% of the solid
xylitol is melted. As indicated hereinabove, in each of the
embodiments in the present process, in the extruder, not all of the
solid xylitol is melted, that is, less than 100% of the solid
xylitol is melted.
[0057] It is essential that not all of the xylitol in the
composition is melted. As explained hereinbelow, the product
contains crystals of various sizes. Some are large and others are
small. If all of the xylitol in the extruder composition is melted,
then upon cooling, recrystallization will occur, creating the
problems described hereinabove, which problems are to be avoided.
If the xylitol crystallizes in the extruder, it causes the
apparatus to be clogged.
[0058] The partial melting of the extruder composition in the
extruder is effected at a temperature and for sufficient amount of
time so that only a portion of the solid is melted, as described
herein. In an embodiment, the temperature of the extruder
composition in the extruder ranges from about 190 F. to about 205
F. and in another embodiment from about 194 to about 200 F. The
temperature at which the extruder is to be set so that the slurry
is in this temperature range is easily determined by one of
ordinary skill in the art.
[0059] By "slurry", it is meant a translucent mass in a slushy like
state. As a slurry, it contains a heterogeneous mixture of the
ingredients described hereinabove in solid and liquid form. For
example, it comprises xylitol solid mixed in with xylitol liquid
and any optional ingredients. As indicated below, the mixture
remains a slurry and is not completely melted in the extruder.
[0060] The partial melting is effected in the extruder. It can be a
single screw extruder, a twin screw extruder or multi-screw
extruder, commonly used in the confectionery arts. The extruder may
have various temperature zones. Generally, the various temperature
zones are sufficiently high as described above, to effect the
formation of the slurry and to achieve a partial melting of the
xylitol therein. The extruder composition in the extruder is at a
temperature sufficiently high so that the composition is partially
melted but sufficiently low so that it does not all melt. In
addition, in the exit zone (also known as the discharge zone), the
temperature thereof is sufficiently high so that the partial melt
is maintained, and sufficiently low so that the xylitol does not
all melt. In an embodiment, the slurry in the exit zone of the
extruder is at a temperature ranging from about 190 F. to about 205
F., and in a still further embodiment, from about 194 F. to about
200 F.
[0061] In the partial melting step, the mixture is in a partial
molten state, forming a slurry and remains in the slushy state. The
mixture is maintained at the appropriate temperature range at or
about the melting point of xylitol for a sufficient amount of time
to form a slurry and maintain the consistency of the slurry in a
slushy state in and through the extruder and subsequent processing.
If the temperature of the slurry is too low, then the slushy
mixture would result in rapid crystallization and uncontrolled
hardening of the slushy mixture and possible clogging of the
equipment. If the temperature of the slurry is too high, then more
of the slush may melt and the slushy state may not be
maintained.
[0062] The slurry may be further processed to form the desired
product by methods commonly used in the confectionery industry, for
example, depositing or molding. However, prior to being molded or
deposited, the slurry, in one embodiment, is transferred to the
depositor. A predetermined amount of the slurry, such as in the
form of a drop or sheet, is deposited onto a belt, in another
embodiment, the slurry is placed into a mold. However, prior to
reaching the mold or prior to the extruded composition being
deposited onto a belt, the slurry is maintained at a temperature so
that it remains a slurry. In an embodiment the slurry is maintained
at or about the same temperatures as when present in the exit zone
or as it exits from the extruder. In an embodiment, the slurry is
maintained initially, after it exits the extruder at about 190 F.
to about 205 F. and in another embodiment, about 194 F. to about
200 F. by conventional methods known to one of ordinary skill in
the art, such as by jacketing the equipment with heating means.
[0063] In carrying out the process, the mixture in an embodiment is
maintained in a relatively dry atmosphere to prevent moisture pick
up such that the moisture content does not exceed about 1%
moisture.
[0064] This process of the present invention is described
hereinbelow in greater detail by referring to the drawings. The
extruder contains a feeding device, for example a feed hopper or
feed screw, at least one outlet in the discharge zone from which
the extruder composition leaves the extruder and in between, an
extrusion barrel connecting the feed hopper to the outlet and which
contains mixing and kneading regions and means of thermal
regulation of the mixing and kneading regions to control the
temperature of the mixing regions.
[0065] An example of an extruder (12) for use in this invention is
depicted in FIG. 1. It is a single screw extruder and it has a
vertical feed screw (15) which forces the extrusion composition
into the extrusion section (16) of the extruder (12). FIGS. 2a, 2b
and 2c illustrate cross-sectional views of the of the extruding
section of a single screw extruder (12). A depicted in FIG. 2a, the
extrusion section of a single-screw unit is driven by a central
longitudinal shaft 21 onto which screw segments 22 and steamlocks
23 are affixed to the shaft (See FIG. 2b). The screws 22 and
heating means, e.g., electric resistors or heating systems operated
by induction or steam, are affixed. In FIGS. 2a, 2b and 2c, the
heating means is a heating system operated by steam. The steamlocks
23 are arranged to provide a progressively tighter pitch and
greater resistance from the inlet zone to the outlet zone. This
arrangement results in the development of a continually increasing
pressure gradient. The barrel segments 24 (FIG. 2c) are
consecutively affixed onto the extruder housing and are jacketed to
receive either steam or cooling water. These jacketed barrels
assist in the development and control of the temperature in the
extruder. Each screw segment 25 is positioned within a
corresponding barrel segment 24 to make up a designated zone. The
shaft 21 revolves at variable speeds within the barrel to establish
the required shearing conditions.
[0066] The extruder as shown can have a number of temperature
zones. The embodiment depicted in FIG. 1 has six zones in a
single-screw extruder. Each zone is provided with a separate double
jacket. The first zone in the extruder 12 is the inlet zone and the
last zone is the discharge or exit zone. The inlet zone contains a
wide flight tapered screw designed to direct the feed mass into the
barrel housing. Zones two, three, and four desirably have screws
with intermediate flight spacings intended to convey and compress
the mass. Zones five and six are equipped with "tight flight"
screws. The tight flight screws work and compress the mass. The
discharge zone includes an exit die head. The exit die head
contains multiple hole outlets to release the extruded mass to the
atmosphere.
[0067] The extrusion composition is charged into the inlet zone of
the extruder 12. Due to the extremely high total surface area and
low moisture content of the extruder composition,
particle-to-particle friction caused by the mechanical shear of the
rotating screw shaft 21 generates sufficient heat to rapidly
increase the temperature of the mass in the extruder barrel. If the
mass is heated up too quickly, various feed-flow problems,
including the possibility of material blow-back, can occur.
[0068] In FIG. 2 zones two and three are water-cooled jackets that
decrease the rate of temperature rise of the extruder composition
and prevent the problems described hereinabove in the background of
the invention. Even with these water-cooled jackets, the
temperature of the extrusion composition in the extruder is
sufficient to maintain the xylitol as a slurry, i.e., a mixture of
molten xylitol and crystalline xylitol. In an embodiment, the
temperature of the slurry is maintained about the melting point of
xylitol, e.g., about 190 to about 205 F., while in an embodiment
from about 194 to about 200 F. However, the temperature of the
extruder is increased from friction within the extruder barrel. The
extrusion composition is kneaded in zones two and three and
conveyed to zone four. In the extruder e.g., in zone four, the
extruder composition is compressed and further heated, but the
extrusion composition is and remains a partial melt, a slurry.
Zones four, five, and six have steam-heated jackets that may,
correspondingly, increase the amount of liquid phase, but the
extruder composition still remains a partial melt. The temperatures
of zones four and five are usually controlled.
[0069] In another embodiment, the extruder is a twin-screw type
extruder. In this embodiment, it has a feed hopper, as in the
single screw extruder. It is a mixing device which kneads the mass,
but instead of having one screw, it contains a twin screw system.
It may optionally have an outlet die. But it also contains a means
of thermal regulation similar to that depicted in FIG. 1. The
starting material introduced into the mixing area is subjected to
shearing forces and intense mechanical friction by the compression
in the turns of the screw and at the same time to heating which is
introduced by the heating means.
[0070] The twin screw extruder has heating zones, and the
temperatures of the slurry in the various zones, including the
discharge zone, are as described for the single screw extruder,
discussed hereinabove. Again, as in the single screw extruder, the
temperature of the slurry in the various temperature zones and in
the discharge is at a temperature in which the xylitol forms a
slurry and is maintained as a slurry. This, in one embodiment the
temperature ranges from about 190 F. to about 205 F., and in a
further embodiment, from about 194 F. to about 200 F.
[0071] Nevertheless, regardless of the type of extruder, the
xylitol in the composition in the extruder and throughout the
extruder and discharged from the extruder is only partially melted.
As stated above, the extruder composition is not completely
melted.
[0072] Next, the slurry discharged from the extruder is formed into
the desired shape and then cooled. As described below it can any
shape that is desired. For example, it may be pastilled, deposited
on a belt, molded, or sheeted to form solid product of suitable
size and shape. For example, the slurry may be extruded from the
extruder, into a depositor, as described above. The bottom of the
depositor has a mechanism to control the flow of materials
therefrom, thus allowing it to be metered at a desired rate. For
example, the area of the depositor contains pistons through which
the slurry is fed and deposited onto as belt at a desired rate.
[0073] Reference is made to FIG. 3. FIG. 3 depicts the extruder
discharging the slurry onto a hopper, which is part of the
depositor. The depositor contains a plurality of pistons set
parallel. The pistons are arranged so that the nozzles thereof pass
through a manifold. The slurry is conveyed to the pistons.
[0074] While in the depositor, including the hopper, the partially
melted slush is maintained as a partial melt. For example, it is
maintained at a temperature ranging from about 190 to about 205 F.
and in another embodiment from about 194 to about 200 F. Although
not shown, the depositor, (including the hopper and the area around
the pistons) is jacketed with heating means, as described above
with the extruder.
[0075] The pistons work with the nozzles to assure a set amount in
the form of a drop is deposited onto the belt or into a mold.
Depositing the xylitol slush directly onto a belt produces a
desirable rounded candy piece. In an embodiment, it produces a
rounded candy piece (sphere) when the belt on which it is deposited
has a contact angle above about 110.degree. and less than about
180.degree.. By contact angle, it is meant the angle at the point
where the outside surface of the slurry from the depositor
intersects or meets the belt. In another embodiment, the contact
angle ranges from about 120.degree. to about 180.degree. and in
another embodiment from about 135.degree. to about 180.degree..
[0076] The slurry discharged from the extruder may be deposited
onto a belt or into a mold to form a solid product of suitable size
and shape. In an embodiment, the slurry extruded from the extruder
is deposited into molds having suitable shapes and sizes.
[0077] When placed into a mold, the slurry is cooled to a
temperature where the slushy composition is a temperature at which
it solidifies, e.g., it is below the temperature of 190 to about
205 F. to allow the xylitol contained therein to harden.
[0078] The final product from the mold or belt may be formed into a
variety of shapes that include, but are not limited to spheres
(discs), hemispheres, cubes, cuboids, pyramids, squares,
rectangles, triangles, octagons, hexagons, pentagons, prisms, or
any yertz, which is an elliptical cylinder which is wider at the
top than at the bottom or any other desired shape. A picture of the
yertz shaped product is depicted in FIGS. 6a-6c. Alternatively, the
final product from the mold or belt may be formed into an irregular
shape.
[0079] Once the mixture is formed into the desired shape, the
formed product is cooled. This can be effected, for example, by
allowing the temperature of the slushy material to fall below the
melting point of xylitol, for example, below about 190 F.
Temperatures as low as ambient temperatures may be used to cool the
slurry to crystallize it. For example, the slurry may be passed
through one or more cooling tunnels to gradually cool the formed
product to room temperature. In an embodiment of the present
invention, air is employed as a cooling medium. Air used for
cooling should not be too cold to avoid sweating. In an embodiment
of the invention, the temperature of air is between about 68 F. and
about 104 F.
[0080] In another embodiment, air at a temperature of less than
about 190 F. is utilized to cool the final product. That is, the
product is allowed to stand until it completely solidifies. The
cooled solidified product may optionally be grinded to whatever
size desired.
[0081] In the present process, once the temperature of the slurry
is below about 190 F., it takes less than about ten minutes for the
xylitol in the composition to completely solidify. In another
embodiment, it takes less than five minutes for the xylitol in the
composition to completely solidify once the temperature is lowered
to less than 190 F., while in another embodiment it take about two
to about three minutes to solidify.
[0082] The formed comestible product is then packaged. Conventional
packaging materials and methods can be used for packaging the
comestible product of the present invention based on the size and
shape of the comestible product.
[0083] It is to be noted that the percentage by weight of the
composition of the present invention remains about the same
throughout the process. Thus, for example, if the mixture in the
first step contains about 60% xylitol, the mixture in the slurry
contains xylitol at about 60% by weight and the final product
contains about 60% by weight.
[0084] The moisture content throughout the process remains at about
constant. More specifically, in an embodiment, the moisture content
is less than about 1% by weight, and in another embodiment, is less
than about 0.50% by weight and in a still further embodiment is
less than about 0.25% by weight.
[0085] The product formed from the present process comprises at
least 60% xylitol by weight. It has a low moisture content, less
than about 1% by weight. Further, the dissolution rate of the
product formed by the present process is dependent upon many
factors, including the shape and weight of the product and the
temperature of the solvent, usually water, in which the dissolution
rate is determined. By dissolution rate, it is meant as the time
required for predetermined amount, such as 0.75 gram, to completely
dissolve. Although the product may be any shape or size, for
purposes of describing a characteristic of the product, a 0.75 gram
piece, when molded into the shape of the yertz, as shown in FIGS.
6a-6c, having the following dimensions: a base width of 8.20 mm, a
base length of 13.26 mm, a height of 8.71 mm, an angle of
10.degree. between the vertical axis and the side (that is, the
angle between the base and the side is 80.degree.) and 0.25 mm
radius fillet, has a break pressure point of less than about 110
MPa. In one embodiment, the average break pressure of such as piece
ranges from about 30 to about 105 MPa, and in another embodiment,
from about 40 to about 100 MPa. The dissolution rate of this sample
in a 37 C. bath of water ranges from about 200 seconds to about 400
seconds, and in another embodiment from about 250 seconds to about
350 seconds and in another embodiment, from about 290 seconds to
about 320 seconds.
[0086] The product formed from the present process is quite unique.
It has irregularly shaped crystals. It is comprised of crystals of
various sizes, wherein the size of the larger crystals is
substantially larger than the size of the smaller crystals. In an
embodiment the larger crystals range from about 400 to about 600
micrometers. These various sized crystals are randomly dispersed
throughout the product. Because of the various crystal sizes and
the looseness of the crystals in the product, the product of the
present invention is not very hard. The presence of the large size
crystals makes the comestible product of the present invention
breakable without significant effort. When placed in the mouth of
the consumer, the comestible product of the present invention melts
rapidly and the consumer feels the cooling effect and flavor more
readily than if the same product was prepared by conventional
methods in which the xylitol is completely melted and then
recrystallized. Further such a product prepared by the latter
method is substantially harder than the product prepared by the
present process.
[0087] In an embodiment, the comestible product of the present
invention is substantially free of any sugar alcohol other than
xylitol. Examples of the alcohols that the comestible product is
substantially free includes glycol, glycerol, erythritol, threitol,
arabitol, ribitol, mannitol, sorbitol, dulcitol, iditol, isomalt,
maltitol, lactitol, polydextrose, polyglycerol, and the like. It
contains at most trace amounts of flavorants containing those sugar
alcohols. The comestible product is substantially free of and in an
embodiment does not contain any aldoses and ketoses, including
sugars, such as glucose and sucrose and contains .ltoreq.2%
Maltodextrin having a DE of less than 20. In another embodiment,
the present composition is substantially free of maltodextrin,
(.ltoreq.1%).
[0088] The product formed is non-compressible and is preferably not
a tablet, although it can be in the shape of a tablet. Therefore,
no binding agent or lubricant is present in the composition. It has
a crunchy texture. By non-compressible it is meant that the product
will break into pieces if compressed.
[0089] The product produced may be used as a pharmaceutically
active compound. As employed herein the term "pharmaceutically
active compound" refers to an organic or inorganic orally
ingestible compound which is taken for medicinal, dietary and
nutritional purposes and which is particulate in form. As described
hereinabove, xylitol has several beneficial features in dental
hygiene. Thus, in one embodiment, the comestible product is a
pharmaceutical composition comprising a pharmaceutically effective
amount of xylitol. As indicated hereinabove, in an embodiment the
product contains at least about 80% by weight xylitol. The
pharmaceutical composition also contains excipients normally found
in the pharmaceutical arts.
[0090] Alternatively, the comestible composition comprises a
pharmaceutically effective amount of as pharmaceutically active
compound and excipients normally found in the pharmaceutical arts
present together with the xylitol. Many drugs, such as aspirin,
when placed in the mouth dissolve, leaving a horrible taste in the
mouth. By adding a pharmaceutical to the present composition, it is
much easier to ingest because the present composition masks the
flavor of the pharmaceutical and makes the taste pleasant because
of the cooling effect of the present composition. Any
pharmaceutical may be utilized, as long as it does not decompose
under the process conditions utilized. The drugs utilized are
NSAIDS, over the counter drugs and prescribed drugs. Examples
include, but are not limited, to pain relievers, such as
salicylates: aspirin (also called acetylsalicylic acid or ASA),
choline salilcylate, magnesium salicylate, and sodium salicylate
and the like; acetaminophen; nonsteroidal antiinflammatory drugs
(NSAIDs: ibuprofen, naproxen sodium, and ketoprofen), and the like;
antihistamines, such as, loratadine, brompheniramine,
chlorpheniramine, dimenhydrinate, doxylamine, and the like;
decongestants, such as pseudophedrine, phenylephrine, and the like;
laxatives, including bulk forming laxatives such as
methylcellulose, polycarbophil, psyllium, and the like; stool
softener laxatives, such as docusate sodium and the like; saline
laxatives, containing non-absorbable ions, such as magnesium,
sulfate, phosphate and sodium and the like, e.g., magnesium
hydroxide, magnesium citrate, sodium phosphate and the like;
stimulant laxatives, such as, bisacodyl, sodium bicarbonate and
potassium bitartrate, sennosides, senna, and the like; antimetics,
such as meclizine hydrochloride (Bonine), dimenhydrinate
(Dramamine) and the like; oral nasal decongestants, such as
drixoral nasal decongestants and the like; cough suppressants, such
as dextromethorphan, guaifenesin, and the like; vitamins and
minerals; antidiarrheal such as adsorbents, e.g., attapulgite,
polycarbophil, and the like; anti-motility antidiarrheal, such as
loperamide (Imodium) and the like; bismuth compounds, such as
bismuth subsalicylate (Pepto-Bismol), and the like; drugs for
treating acid ingestion, such as simethicone (Phazyme; Flatulex;
Mylicon; Gas-.X; Mylanta Gas), activated charcoal, and the
like.
[0091] If an additional pharmaceutically active agent is to be
present, it is prepared as described above for the comestible
product. In one embodiment, the pharmaceutical is an analgesic,
e.g., aspirin. The pharmaceutically active agent is blended with
solid xylitol and with any other pharmaceutically acceptable
excipients that are normally used and the mixture is then put into
an extruder as described above. In this embodiment, the xylitol is
the pharmaceutically acceptable carrier. As described hereinabove,
the xylitol in the composition is partially melted in the extruder.
The parameters discussed above for the extruder are applicable
here, including the temperature of the extruded composition slurry
in the discharge zone and as the slurry exits the extruder. In
other words the temperature of the slurry in the exit zone ranges
from about 190.degree. F. to about 205.degree. F. and in another
embodiment from about 190.degree. F. to about 200.degree. F. Once
the slurry is discharged from the extruder, it may be deposited,
molded or pastilled. Subsequently, it is cooled and optionally
milled to the desired size. The composition contains the medicament
in effective amounts. The composition contains up to about 40% by
weight of the pharmaceutically active compound and up to about 60%
xylitol. For example, in an embodiment it contains as little as
0.01% medicament up to about 40% by weight medicament and in
another embodiment from about 1% to about 38% by weight medicament.
In such embodiments, the amount of xylitol ranges from about 60% up
to about 99.99% xylitol and in another embodiment from about 62% up
to about 99% by weight of the composition.
[0092] Unless indicated to the contrary, the term "extruder" and
"extruder apparatus" are synonymous and are used interchangeably.
In addition, the exit zone of the extruder and the discharge zone
of the extruder are synonymous and are used interchangeably.
[0093] Further, unless indicated to the contrary, all percentages
are by weight of the composition.
[0094] Further, the plural denotes the singular and vice versa.
[0095] In addition, the terms "slurry" and "slush" and "slushy
state" are being used interchangeability. These terms are meant to
be synonymous.
[0096] Furthermore, the term "extrusion composition" refers to the
composition that is put into the extruder.
[0097] The terms "extruder" and "extrusion apparatus", as used
herein, are synonymous, and are being used interchangeably.
[0098] The term "substantially free", as used herein refers to the
composition not containing a particular component or a very small
amount, but if present, it does not affect any of the properties
described herein. For example, in an embodiment, if the composition
is substantially free of a component, refers to the component being
present in less than about 2% by weight and in another embodiment
less than about 1.0% and in another embodiment, less than about
0.1% by weight.
[0099] Unless indicated to the contrary, it is to be understood
that the temperatures are in F.
[0100] The following examples further illustrate the present
invention. They are not meant to limit the present invention.
EXAMPLE 1
[0101] Granular xylitol (98.8% w/w), powdered cooling compound
WS23(N,2,3-trimethyl-2-(1-methylethyl) butanamide (0.2% w/w) and
granular peppermint flavor (1% w/w) were dry blended in a small
batch mixer at ambient temperature of about 65 F.-75 F. The dry
blending continued until at homogenous mixture was obtained. The
dry blend mixture was then fed into a water jacketed cooled hopper
which feeds the product into a single screw extruder (Wayne,
Totowa, N.J. having a 24:1 L/D ratio, 1 inch diameter screw in a
3:1 compression ratio). The extruder has five temperature
controlled zones through which the mixture passed. The temperature
in the various zones was set at about the melting point of xylitol,
and the discharge of the extruder was a 40% melted mass at 198 F.
The mass was solidified in a mold in the shape of mold within 2-3
minutes after being placed into a mold that was then exposed to
ambient air temperature. The product produced was a soft hard candy
in the shape of a mold that was easily broken by biting into
it.
EXAMPLE 2
[0102] Granular xylitol (98.8% w/w), powdered cooling compound WS
23 (0.2% w/w) and granular peppermint flavor (1.0% w/w) were dry
blended at ambient temperature of about 65 F.-75 F. The dry blended
mixture was fed into the single screw extruder described in Example
1. The extruder is temperature controlled in five zones, each
temperature of the composition in each zone being about the melting
point of xylitol. The discharge temperature of the product exiting
from the extruder was about 196 F. The product discharged from the
extruder was about 40% melted. The product, which was a slush, was
gravity drained into a heated depositor hopper that maintained the
xylitol near the melting point range of the xylitol, which is about
197.6-204.8 F. The product was then deposited onto a conveyer belt
where it took about 2-3 minutes to solidify when exposed to ambient
air temperature. The product is softer than a typical hard
candy.
EXAMPLE 3
[0103] This example measures the dissolution rate of samples.
[0104] The following equipment was used:
[0105] 1. 1000 mL Pyrex glass beakers [0106] 2. Octagon shaped PTFE
coated 2'' magnetic stir bar with molded-on pivot ring [0107] 3.
VWR Advanced Multiposition Stirrer--Four position stir plate with
adjustable speed controlled for all positions simultaneously by
integral knob--Catalog #12621-022 [0108] 4. Thermometer--Mercury
filled, partial immersion (76 mm immersion), 0 C. to 200 C
range--calibrated against NIST traceable digital thermometer [0109]
5. Three position digital timer [0110] 6. Deionized water [0111] 7.
Balance, analytical--range: 0-200 gram, sensitivity .+-.0.0001 gram
[0112] 8. Balance, top loading electronic--range 0-3000 g,
sensitivity .+-.0.01 gram. [0113] 9. Hot plate [0114] 10. 4 Liter
Pyrex glass Erlenmeyer flask
[0115] Deionized water was heated in 4 Liter Erlenmeyer to 37 C.
600 grams of the heated water was divided into three separate 100
mL glass beakers. Stir bars were placed into the beakers. The
beakers were positioned on three positions of the Four position
stir plate.
[0116] The speed was adjusted using digital control to 200
revolutions per minute. The water temperature at the start and end
of the dissolution procedure was recorded.
[0117] When a pre-weighted sample piece was dropped into each
beaker, the timer was started.
[0118] When the entire piece visibly dissolved the elapsed time was
recorded as dissolution time.
[0119] The procedure was repeated each time using clean beakers and
fresh 37.degree. C. water.
[0120] The results for three samples prepared as above are depicted
below:
TABLE-US-00001 Avg % Std Dev No. Avg % Std Sam- Dissolution for
Dissol. Measure- Sample Dev for Pc ples Rate (s) Rate ments Wt Wt
Shape 1 293 6% 4 0.7237 1.40% yertz 2 582 7.70% 4 0.8296 7.20%
yertz 3 650 .sup. 12% 4 0.7505 7% yertz
[0121] The first sample (Sample 1) is the product of Example 2
described herein above. The second sample (Sample 2) is a sugar
hard candy having a 60/40 Sugar/CS ratio:
[0122] The third sample (Sample 3) is an isomalt/HSH sugar-free
hard candy.
EXAMPLE 4
[0123] The moisture content was measured using the Karl Fischer
titration method using a Brinkman Karl Fischer Titrator with
homogenizer and dissolving the samples in a methanol formanide
solution (3:1).
[0124] The water activity was measured as follows. Using a
Instrumentation: Decagon Aqualab water activity meter connected to
a computer running Aqualink Report Generator (Decagon Devices,
Inc., Pullman, Wash.), the water activity was measured as follows:
[0125] (a) Standardizing measurement: A slush of potassium chloride
crystals in distilled water is prepared such that the solution is
saturated with potassium chloride and potassium chloride crystals
are visible on the bottom of the saturated solution. This was
equilibrated to room temperature and then placed into a small cup
that was inserted into the drawer and placed into the instrument.
The reading is adjusted to be 0.859 at 15 C., 0.851 at 20 C., 0.843
at 25 C. or 0.836 at 30 C. (L. Greenspan. 1977. J. Res. NBS--A.
Physics and Chemistry, 81A(1):89) according to the reported
temperature. [0126] (b) Sample measurement: The instrument was set
to report readings continuously. The sample is placed into a cup
placed into the instrument. The water activity is reported as the
value which does not change by more than 0.002 units between
subsequent readings.
[0127] Using samples prepared in accordance with the present
process described herein, the water activity of the samples was
measured as follows:
TABLE-US-00002 Water Samples Moisture Activity at 20 C. 4 0.24%
0.59 5 0.26% 0.50
BACKGROUND FOR EXAMPLES 5-8 AND COMPARATIVE EXAMPLE 1
[0128] The procedure for measuring, the texture is as follows:
[0129] Equipment: The equipment that was used was TA.XT2i (Stable
Micro Systems, Ltd., Scarsdale, N.J.) fitted with a 30-kg measuring
head with a maximum force reading of 36800 g. Pieces were placed on
a raised platform (HDP/90 heavy duty platform, Stable Micro
Systems, Ltd., Scarsdale, N.J.) set upon the top of the base of the
instrument.
[0130] Piece shapes; The "beltDep" piece is formed in the shape of
a disc (sphere) by depositing slush directly onto a room
temperature belt which progressed through a cooling tunnel
resulting in a piece with average height of 4.17 mm (standard
deviation of 0.13-mm) and average weight of 1.00-g (standard
deviation of 0.036-g). The "Yertz" piece is formed by depositing
slush directly into an oval-cylinder piece with slanting sides
(narrower at the bottom of the mould than the top) with a mould
bottom that was flat and 5-mm across the narrow oval axis. The
mould was scraped to remove excess slush immediately after filling
before hardening. The average height is 8.79 mm (standard deviation
of 0.11 mm) and average weight of 0.746 g (standard deviation of
0.014 g). The "mouldDep" piece is formed by depositing slush
directly into a mould with a concave bottom resulting in a piece
that is flat on the mould-free side and convex on the top. The
average height is 5.3 mm (standard deviation of 0.66-mm) and the
average weight was 1.46 g (standard deviation 0.22 g).
[0131] Fixtures A 2 mm blunt cylinder (2 mmBlunt) (part P/2, Stable
Micro Systems, Ltd, Scarsdale, N.J.) with 3.1615 mm.sup.2 area
beveled blade (knife/guillotine blade of HDP/BS Blade set, Stable
Micro Systems, Ltd., Scarsdale, N.J.) (bevelBlade) with 0.5-mm
width of the flat area of the blade for contact with the sample The
blade contact area is 0.5 mm times the length of the blade
contacting the sample.
[0132] The procedure was as follows:
[0133] 0.1 mm/s to a distance or strain that results in the piece
breaking, withdrawn at 10-mm/s, recording 200-pts/s. The beltDep
was oriented with the belt-side down and compressed with the 2 mm
blunt probe. The yertz was oriented with the mould-free side
face-down on the platform and the probe was placed on the
flat-bottom-mould face. When using the beveled blade, the blade was
oriented across the narrowest axis of the oval which resulted in a
contact area of 5 mm long by 0.5 mm wide or 2.5 mm.sup.2 area. The
mouldDep was oriented with the flat-mould-free face against the
platform and the 2 mm-blunt probe was oriented at the apex of the
convex top.
[0134] Analysis: maximum force at failure. The force in grams was
converted to pressure in MPascals by first dividing by the area of
contact and then converting to MPascals by multiplying by
0.009807.
[0135] Software data collection: Texture Exponent (Stable Micro
Systems, Ltd., Scarsdale, N.J.)
[0136] Statistical analysis: Excel (Microsoft, Redmond, Wash.).
Within a dataset, "min" and "max" are the minimum and maximum
pressure observed, respectively. "Average" is the average value,
while "median" is the 50.sup.th percentile number when ranked from
least to greatest. "STD dev" is the standard deviation of the data
set and "95 CI" is the half-width of the 95% confidence interval
for the dataset based on the standard deviation and 2-tailed
t-distribution with the degrees of freedom of that dataset. "95UL"
is the estimated the upper limit for 95% of all values represented
by this dataset which is the sum of the average and 95CI.
EXAMPLE 5
[0137] Xylitol with flavor was partially melted in a single screw
extruder and the slash was formed into yertz-shaped pieces that
were average 8.8 mm height and 0.75 g weight. The pieces were
demoulded and tested 45 min, 25 hr, 7 day and 101 days after
pouring into the mould. The resulting break-pressures were
observed.
TABLE-US-00003 Observed break pressure of yertz shape from slush
formed on a single screw extruder break pressure number observed
Mpa 45 min 25 hr 7 day 101 day <10 0% 0% 0% 0% <20 0% 0% 0%
0% <30 5% 0% 0% 0% <40 40% 12% 1% 3% <50 40% 33% 6% 10%
<60 13% 45% 30% 17% <70 2% 11% 27% 22% <80 0% 0% 17% 33%
<90 0% 0% 15% 13% <100 0% 0% 3% 3% >100 0% 0% 0% 0% count
110 110 110 72 min, MPa 21.1 30.2 38.6 35.5 max 61.1 67.3 91.8 93.5
average 41.3 50.3 65.7 67.8 median 41.0 51.2 64.2 69.6 std dev 7.6
8.4 12.1 12.5 95CI 15.0 16.6 23.9 24.9 95UL 56.30 66.88 89.59
92.73
[0138] The data of Table 1 indicates that the average
break-pressure does not change after the first 7 days after
forming. The data indicates that 95% of individual piece
break-pressure will be less than 93-MPa after 101 days. This is
about 1/10.sup.th of the hardness of dentine.
EXAMPLE 6
[0139] Xylitol with some flavor and color was partially melted in a
single screw extruder and the slush was fed into the hopper of a
depositor, from which slush was deposited into the yertz mold.
Break pressure was determined on the demoulded yertz pieces 45
minutes, 1 day and 7 days after depositing.
TABLE-US-00004 Observed break pressure on xylitol- flavor slush
formed in a single screw extruder, transferred to a depositor
hopper and then depositted into a yertz mould peak proportion
pressure observed range, MPa 45 m 1 d 1 w <20 0% <30 10%
<40 33% 0% <50 43% 20% 0% <60 11% 40% 40% <70 2% 40%
40% <80 1% 0% 0% <90 0% 20% >90 0% count 82 10 10 min, MPa
26.9 42.7 50.6 max 73.7 69.2 88.3 average 41.7 57.1 64.0 median
40.3 57.9 60.6 std dev 8.2 9.4 12.2 95CI 16.3 21.2 27.5 95UL 90.0
90.4 115.9
[0140] After 1 week, the average break-pressure is no different
than the mould were filled with slush directly from the single
screw extruder. Based on the number of observations, 95% of pieces
are expected after 1 week to have a break-pressure less than 116
MPa. With a larger number of observations as obtained in Example 1,
it would be reasonable to reduce this 95UL to that of Example 5
since the standard deviation and average are essentially the same
at 1 or more weeks.
EXAMPLE 7
[0141] Xylitol-flavor slush was formed using the single-screw
extruder and poured into three different moulds. The demoulded
pieces were tested for break-pressure at ages between 7 and 27
weeks using either the 2-mm blunt probe or the beveled blade.
TABLE-US-00005 Comparison of xylitol pieces from single screw
extruder made in different shapes and analyzed by two different
probes formula shape test xylitol xylitol xylitol xylitol xylitol
age beltDep beltDep yertz yertz mouldDep break 2 mmBlunt 2 mmBlunt
2 mmBlunt bevelBlade 2 mmBlunt pressure 10 wk 7 wk 27 wk 27 wk 23
wk <10 MPa 0% 0% <20 MPa 6% 0% <30 MPa 36% 30% 0% 0%
<40 MPa 20% 30% 5% 0% 5% <50 MPa 18% 16% 15% 5% 30% <60
MPa 12% 10% 35% 0% 45% <70 MPa 4% 6% 35% 35% 20% <80 MPa 4%
4% 10% 30% 0% <90 MPa 0% 2% 0% 25% <100 MPa 0% 2% 5% >100
MPa 0% 0% 0% count 50 50 20 20 20 min, MPa 17.2 21.0 37.9 42.8 34.4
max 74.8 96.1 71.9 97.3 66.7 average 37.0 41.5 57.3 73.3 52.7
median 34.5 38.4 57.9 72.1 53.1 stdev 14.6 16.7 9.3 11.2 8.0 95CI
29.3 33.6 19.4 23.5 16.7 95UL 66.2 75.1 76.7 96.8 69.4
[0142] The data indicate that there is some discrepancy between the
2 mm blunt probe and the beveled blade, with the estimated 95UL
being slightly less for the 2-mm blunt probe. The data indicate
that piece shape does not affect the 95UL break-pressure which
remains under 80 MPa for the 2-mm blunt probe regardless of
shape.
EXAMPLE 8
[0143] A xylitol/flavor slush was formed using a twin-screw
extruder and extruded into two different shapes. Each type was
tested for break-pressure using two different fixtures. The yertz
shape was tested using the beveled blade and the molded deposit was
tested using the 2-mm blunt probe.
TABLE-US-00006 Observed break pressure on two different shaped
pieces fromed by slush made by a twin-screw extruder shape test
yertz age bevelBlade break break discMould pressure 1 wk pressure 2
mmBlunt MPa frequency MPa 8 mo <40 0% <40 5% <60 5% <60
25% <80 50% <80 65% <100 18% <100 5% <120 23%
<115 0% <145 5% >115 0% >145 0% count 22 20 min, MPa
49.0 49.3 max 144.3 82.7 average 84.8 63.2 median 78.6 62.8 std dev
23.4 12.9 95CI 48.7 27.0 95UL 133.5 90.2
[0144] The data indicate that the twin-screw extruder formed pieces
that had a higher 95UL break-pressure than those formed using the
single-screw extruder. The estimated 95UL break-pressure is 30 and
20 MPa higher for beveled blade and 2-mm blunt probe fixtures,
respectively.
COMPARATIVE EXAMPLE 1
[0145] Hard candy both sugar and sugar-free described in Example 3
was formed into two different mould shapes and then tested with
either the beveled blade or the 2-mm blunt probe. The maximum
pressure observed for the beveled blade and 2-mm blunt probe was
144 and 115 MPa respectively, due to the limitations of the TA.XT2i
30-kg sensing head.
TABLE-US-00007 Sugar or Sugar-free hard candy was formed into
either the yertz or moulded disc (discMould) and tested by two
different test fixtures formula sugar sugar-free sugar shape yertz
yertz discMould test bevelBlade bevelBlade 2 mmBlunt age 4 d 4 d
break pressure break pressure range, MPa proportion ranges, MPa
<40 0% 7% <40 5% <70 13% 29% <70 0% <100 13% 7%
<100 5% <130 13% 14% <115 5% >130 60% 43% >115 85%
>144 47% 29% count 15 14 20 min, MPa 43 35 33 max >144
>144 >115 average 118 100 109 median 338 106 115
[0146] The data indicate a very wide range of break-pressures for
hard candy that encompasses values beyond the capacity of the
machine. The maximum break-pressure was greater than 144 and 115
MPa when measuring with the beveled blade and 2-mm blunt probe,
respectively. This substantiates that the xylitol/flavor pieces
made with the single-screw extruder have an upper limit
break-pressure that is less than hard candy.
EXAMPLE 9
[0147] Forming piece by depositing on a flat belt. On different
samples of flat belt was placed on 10-20 micro-liter drop of 99.5%
glycerin (USP) which is a model that behaves like the slush
prepared in accordance with the present invention. The contact
angle between the liquid drop and the belt was measured from a
back-lit 0.7-3-fold magnified photograph (Contact Angle System OCA,
Data physics Instruments, GmbH Raiffeisenstra.beta.e, Filderstadt,
Germany) by using a protractor (Acme United Corporation, Fairfield,
Conn.). The left and right side of each of two droplets were
photographed, measured and averaged.
TABLE-US-00008 Belt # contact angle of glycerin drop 1 103 .+-.
1.degree. 2 68 .+-. 1.degree. 3 94 .+-. 1.degree. 4 108 .+-.
7.degree. 5 143 .+-. 7.degree.
[0148] The contact angle of xylitol pieces formed by depositing on
different belt materials were backlit and photographed. The contact
angle was determined as the angle of its side at the point it
intersects its flat bottom. Four pieces were examined measuring the
contact angle on each of four points approximately at points
90.degree. removed from each other around the edge of piece.
TABLE-US-00009 Belt # contact angle of glycerin drop 1 90 .+-.
3.degree. 2 78 .+-. 7.degree. 3 106 .+-. 8.degree. 4 103 .+-.
6.degree. 5 156 .+-. 15.degree.
[0149] From this, depositing xylitol slush directly on a belt
produces a desirable rounded candy piece when the belt on which it
is deposited has a contact angle about 110.degree..
EXAMPLE 10
[0150] The drop-deposited xylitol piece of Example 2, deposited
onto belt #5 of Example 9, was examined using Contact Angle System
OCA, in which the pieces were held on edge using formed aluminum
foil and sidelit using fiber-optic directed light
(KL1500-Electronic, Schott North America, Inc., Elmsford, N.Y.).
The images were then measured against the distance of 1-mm also
imaged under the same conditions.
[0151] The crystal sizes were identified as domains of uniform
light intensity bounded completely by lighter colored lines of
irregular shape. The longest and shortest dimensions were measured
and recorded. A picture of the crystals is depicted in FIG. 4.
[0152] Results: Nine crystals were evident and had the following
dimensions in micrometers. 400.times.180, 280.times.280,
420.times.320, 580.times.320, 210.times.210, 210.times.210,
350.times.140, 170.times.140.
EXAMPLE 11
[0153] The drop-deposited xylitol piece of Example 2 was imaged
along its top essentially looking along the top almost parallel to
surface so as to image the peaks and valleys. The same equipment
was used as in Example 10. The height of the elevations were
estimated from the photomicrographs produced, which is depicted in
FIG. 5.
[0154] As shown in FIG. 5 along the top, peak to trough was
observed to be less than 300 micrometers, while along the side near
the belt, it was observed to be less than 50 micrometers.
EXAMPLE 12
[0155] Granular xylitol (66.3% w/w), aspirin (32.5% w/w) powdered
cooling compound WS23(N,2,3-trimethyl-2-(1-methylethyl) butanamide
(0.2% w/w) and granular peppermint flavor (1% w/w) were dry blended
in a small batch mixer at ambient temperature of about 65 F-75 F.
The dry blending continued until a homogenous mixture was obtained.
The dry blend mixture was then fed into a water jacketed cooled
hopper which feeds the product into a single screw extruder (Wayne,
Totowa, N.J. having as 24:1 L/D ratio, 1 inch diameter screw in a
3:1 compression ratio). The extruder has five temperature
controlled zones through which the mixture passed. The temperature
in the various zones was set at about the melting point of xylitol,
and the discharge of the extruder was at 198 F. The mass was
solidified in a mold in the shape of a mold within 2-3 minutes
after being placed into a mold that was then exposed to ambient air
temperature. The product produced was a soft hard candy in the
shape of a mold that was easily broken by biting into it.
EXAMPLE 13
[0156] The process of Example 12 was repeated, except the amount of
aspirin present was 8% (w/w) and the amount of xylitol was 91.8%
(w/w).
[0157] The above preferred embodiments and examples are given to
illustrate the scope and spirit of the present invention. The
embodiments and the examples described herein will make apparent to
those skilled in the art other embodiment and examples. These other
embodiments and examples are within the contemplation of the
present invention.
* * * * *