Note: Descriptions are shown in the official language in which they were submitted.
BEVERAGE CONCENTRATES WITH INCREASED VISCOSITY AND SHELF LIFE AND
METHODS OF MAKING THE SAME
FIELD
[00021 The disclosure relates to liquid beverage concentrates, and
particularly to shelf
stable viscous concentrates suitable for dilution with a potable liquid for
preparing flavored
beverages.
BACKGROUND
10003] Flavored beverages are widely accepted by consumers and have
increased in
popularity in recent years. Flavored beverages are often prepared at home
using powdered
drink mixes, including commercially-available products like TANG , CRYSTAL
LIGHT , and
KOOL-AID from Kraft Foods, to provide beverages in a variety of flavors,
including fruit and
tea flavors. Some drink mixes require the consumer to add sweetener, typically
sucrose, when
preparing the beverage. Other products that include sucrose often necessitate
that relatively
large amounts of the product be used to prepare each beverage. As the drink
mixes are
provided in dry form, the products generally have a long shelf life. Further,
stability of the
flavor ingredient is not a significant issue because beverages prepared with
the drink mixes are
typically consumed prior to the development of any off flavor notes in the
beverage.
[0004] Flavored beverages may also be prepared from frozen, fruit-flavored
concentrates,
such as those traditionally sold in canisters. These concentrates typically
include a large amount
of water and are generally diluted at a ratio of 1 part concentrate to 3 parts
water to provide the
fruit flavored beverage. These types of products are often susceptible to
spoilage and require
storage at freezer temperatures to provide the desired shelf life.
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[0005] Ready-to-drink flavored water products have also increased in
popularity with
numerous commercial offerings. As these products are provided in diluted form
and are
formulated for direct consumption, there is no additional preparation required
on the part of
the consumer. While these types of products require no preparation time and
may provide
convenience to the consumer in that regard, these types of products are bulky
due to the high
water content and do not allow for the consumer to adjust the amount of flavor
or flavor profile
of the product.
SUMMARY
[0006] The concentrates described herein have increased viscosity which
significantly
improves the stability of certain ingredients despite the liquid concentrates
having a pH that
would be expected to rapidly degrade the ingredients. The concentrates
described herein
advantageously are characterized by reduced production of off-flavor notes and
reduced
degradation of added flavoring, coloring, vitamins, and/or sweetener during
storage at 70 F in
a sealed container as compared to an otherwise identical beverage concentrates
having a lower
viscosity.
[0007] Beverage concentrates contain a greater amount of ingredients per
unit volume than
a dilute, ready-to-drink beverage. By increasing the concentration of
ingredients in the beverage
concentrate, the ingredients more readily come into contact with one another,
which can speed
up rates of reactions that are dependent on acid or oxygen-deterioration
pathways and
ultimately cause the concentrate to have a shorter shelf-life. Many techniques
have been
implemented to slow the rate acid or oxygen-catalyzed reactions, with
encapsulation being one
of these techniques. Encapsulation effectively quarantines sensitive beverage
components away
from solubilized acid or permeating oxygen, thereby reducing the rate of
reaction and
increasing shelf-life. However, not all beverage components have the ability
to be encapsulated
due to physical, chemical, or processing restraints.
[0008] Described herein is a viscous but flowable, liquid beverage
concentrate including a
viscosity increasing agent which provides a highly stable system relative to a
comparative
beverage concentrate with the same ingredients except for at least a portion
of the viscosity
increasing agent such that the comparative beverage concentrate has a lower
viscosity as
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evidenced by a different taste after storage in a closed container at room
temperature after six
months.
[0009] In one approach, a moderately concentrated product may be formulated
to be
diluted by a factor of at least 5 times to provide a final beverage, which can
be, for example, an 8
ounce beverage. In one aspect, the concentrate is formulated to be diluted by
a factor of about 5
to about 15 times to provide a final beverage. In this form, the liquid
concentrate has a pH of
about 1.8 to about 3.1, 1.8 to about 2.9, in another aspect about 1.8 to about
2.7, in another aspect
about 1.8 to about 2.5, and in yet another aspect about 1.8 to about 2.4, in
another aspect about
2.0 to about 3.1, in another aspect about 2.0 to about 2.9, in another aspect
about 2.0 to about 2.7,
in another aspect about 2.0 to about 2.5, and in yet another aspect about 2.0
to about 2.4, and a
viscosity of about 7.5 to about 100 cP, in another aspect about 10 to about
100 cP, in another
aspect about 15 to about 100 cP, in another aspect about 7.5 to about 50 cP,
in another aspect
about 10 to about 50 cP, in another aspect about 7.5 to about 20cP, and in
another aspect about
to about 20 cP, as measured using Spindle SOO at 50 rpm at 20 C with a
Brookfield DVII + Pro
Viscometer. Viscosity in the described range is effective to increase the
stability of flavorings,
colors, vitamins, and artificial sweeteners prone to degradation at the
described pH. In one
aspect, the concentrate includes at least about 0.1 percent acidulant, in
another aspect about 0.1
to about 15 percent acidulant, in another aspect about 0.5 to about 10 percent
acidulant, in
another aspect about 0.75 to about 10 percent acidulant, in another aspect
about 1 to about 10
percent acidulant, in another aspect about 0.75 to about 5 percent acidulant,
and in another
aspect about 1 to about 5 percent acidulant by weight of the concentrate.
[0010] In another approach, a highly concentrated product can be provided
at a
concentration of about 25 to about 200 times, in another aspect about 25 to
about 160 times, in
another aspect about 50 to about 160 times, in another aspect about 75 to
about 160 times, and in
yet another aspect about 75 to about 140 times that needed to provide a
desired level of flavor
intensity, acidity, and/or sweetness to a final beverage, which can be, for
example, an 8 ounce
beverage. In this form, the liquid concentrates described herein have a pH of
about 1.8 to about
3.1, 1.8 to about 2.9, in another aspect about 1.8 to about 2.7, in another
aspect about 1.8 to about
2.5, and in yet another aspect about 1.8 to about 2.4, in another aspect about
2.0 to about 3.1, in
another aspect about 2.0 to about 2.9, in another aspect about 2.0 to about
2.7, in another aspect
about 2.0 to about 2.5, and in yet another aspect about 2.0 to about 2.4, and
a viscosity for a
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Newtonian liquid viscosity of about 7.5 to about 100 cP, in another aspect
about 10 to about 100
cP, in another aspect about 7.5 to about 50 cP, in another aspect about 10 to
about 50 cP, and in
another aspect about 7.5 to about 40 cP, in another aspect about 10 to about
40 cP. If the
concentrate instead has a non-Newtonian liquid viscosity, the viscosity may be
about 7.5 to
about 10,000 cP, in another aspect about 100 to about 10,000 cP, in another
aspect about 50 to
about 10,000 cP, in another aspect about 10 to about 10,000 cP, in another
aspect about 7.5 to
about 5,000 cP, in another aspect about 7.5 to about 1000 cP, in another
aspect about 7.5 to about
500 cP, in another aspect about 7.5 to about 200 cP, in another aspect about
7.5 to about 100 cP,
in another aspect about 7.5 to about 50 cP, and in another aspect about 7.5 to
about 40 cP.
Viscosity is measured using Spindle SOO at 10 rpm at 20 C with a Brookfield
DVII + Pro
Viscometer; however, if the machine registers an error message using Spindle
SOO for highly
viscous concentrates, Spindle S06 at 10 rpm at 20 C should be used. Viscosity
in the described
range is effective to increase the stability of flavorings, colors, vitamins,
and artificial sweeteners
prone to degradation at the described pH. In one aspect, the concentrate
includes at least about
0.5 percent acidulant, in another aspect about 0.5 to about 60 percent
acidulant, in another
aspect about 3 to about 35 percent acidulant, in another aspect about 8 to
about 35 percent
acidulant, in another aspect about 8 to about 30 percent acidulant, about 10
to about 30 percent
acidulant, and in yet another aspect about 15 to about 30 percent acidulant by
weight of the
concentrate.
[0011] The liquid concentrates described herein beneficially include one or
more viscosity
increasing agents to slow the rate of degradation reactions including, but not
limited to,
hydrolysis and oxidation, by increasing the viscosity of the concentrate to a
level effective to
substantially reduce the rate of degradation during storage at 70 F in a
sealed container. It was
surprisingly found that, at least in some cases, rather moderate viscosity
increases were
effective to substantially reduce the rate of degradation reactions of certain
ingredients that are
highly susceptible to degradation despite the concentrates having a relatively
low pH (e.g.,
about 1.8 to about 3.1). The concentrates described herein are particularly
suitable for
ingredients that are highly prone to degradation in acidic solutions,
including for example,
terpenes (such as limonene), sesquiterpenes, terpene alcohol, aldehyde,
terpenoids (such as
citral), betalains, annatto, red beet juice powder, and Vitamins A, C, and E.
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DETAILED DESCRIPTION
[0012] Viscous liquid beverage concentrates are described herein which
provide enhanced
stability to flavorings, artificial and natural sweeteners, vitamins, and/or
color ingredients
despite a substantial water content (e.g., between about 40 to about 98
percent water) and low
pH (e.g., between about 1.8 to about 3.1). The liquid beverage concentrates
described herein
achieve enhanced stability due to increased viscosity. Advantageously, there
is no significant
change in flavor or development of off flavor notes, and no significant change
in appearance
due to color degradation or ingredient browning in the concentrate when stored
at 70 F for at
least about 6 months, in another aspect at least about 9 months, and in
another aspect at least
about 12 months, in a sealed container. In one aspect, the container is light
impermeable when
the concentrate includes light sensitive components. The concentrates
described herein can then
be diluted in a potable liquid to provide flavored beverages with an
acceptable flavor profile
and/or color.
[0013] The concentrates described herein are particularly suitable for
ingredients that are
highly prone to degradation in acidic solutions, including for example,
terpenes (such as
limonene), sesquiterpenes, terpene alcohol, aldehyde, terpenoids (such as
citral), betalains,
annatto, red beet juice powder, and Vitamins A, C, and E. The stability of
these ingredients is
improved in the concentrates described herein.
[0001] Generally it is desirable that the concentrates include acidulant so
that a flavored
beverage made therefrom has a tart flavor that enhances the overall flavor
profile of the
beverage. For example, it may be desirable to provide a lemon-flavored
beverage that has a tart
flavor similar to that of a lemonade drink made with fresh lemons. A variety
of other flavors
can also be enhanced by a tart flavor, such as other fruit flavors. Higher
acid contents are
generally desirable for citrus flavors than for other fruit flavors.
[0014] Accordingly, more concentrated products require a greater quantity
of acidulant to
achieve the same level of acid content in the finished beverage upon dilution.
The acid content
is often detrimental to the stability of various ingredients of the liquid
concentrate. It has also
been found that inclusion of large amounts of water in liquid beverage
concentrates can be
problematic for a number of reasons. Some flavorings, sweeteners, vitamins,
and/or color
ingredients are rapidly degraded in water or in an acidic environment, thereby
limiting the
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types of flavorings that are suitable for inclusion in water-based beverage
concentrates or
ready-to-drink beverages. For instance, some flavor degradation reactions
require the presence
of water while others require protons from dissociated acids. Certain types of
flavorings, such
as acid labile citrus flavorings containing terpenes, sesquiterpenes, terpene
alcohol, and
aldehyde, have greater susceptibility to degradation, and products containing
them typically
have very short shelf lives (even a matter of days) when stored above
refrigeration
temperatures due to development of off-flavor notes and alteration of the
taste profile of the
product. Exemplary other ingredients exhibiting instability in water and/or at
low pH include,
for example, vitamins, particularly vitamins A, C, and E (Vitamin C, for
example, can undergo
browning in an acidic environment), high potency sweeteners (such as, for
example, monatin,
neotame, Luo Han Guo), "natural" colors or other non-exempt colors listed in
the Federal Food,
Drug, & Cosmetic Act (such as for example fruit and vegetable extracts,
anthocyanins, copper
chlorophyllin, curcumin, and riboflavin), sucrose (susceptible to acid
hydrolysis which can then
lead to browning), protein, hydrocolloids, starch, and fiber.
[0015] The liquid concentrates described herein beneficially include one or
more viscosity
increasing agents to slow the rate of degradation reactions including, but not
limited to,
hydrolysis and oxidation, by increasing the viscosity of the concentrate to a
level effective to
substantially reduce the rate of degradation during storage at 70 F in a
sealed container. It was
surprisingly found that, at least in some cases, rather moderate viscosity
increases were
effective to substantially reduce the rate of degradation reactions of certain
ingredients that are
highly susceptible to degradation despite the concentrates having a relatively
low pH (e.g.,
about 1.8 to about 3.1). However, the viscosity of the concentrates is not
increased to the extent
that the concentrates are no longer considered flowable liquid compositions at
70 F.
[0016] As used herein, the term "liquid concentrate" means a liquid
composition that can
be diluted with another liquid, such as an aqueous, potable liquid to provide
a final beverage or
added to a food product prior to being consumed. The phrase "liquid" refers to
a non-gaseous,
flowable, fluid composition at room temperature (i.e., 70 F). The term "final
beverage" as used
herein means a beverage that has been prepared by diluting the concentrate to
provide a
beverage in a potable, consumable form. In some aspects, the concentrate is
non-potable due to
acidulant content and/or flavor intensity. By way of example to clarify the
term
"concentration," a concentration of 75 times (i.e., "75x") would be equivalent
to 1 part
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concentrate to 74 parts water (or other potable liquid) to provide the final
beverage. In other
words, the flavor profile of the final beverage is taken into account when
determining an
appropriate level of dilution, and thus concentration, of the liquid beverage
concentrate. The
dilution factor of the concentrate can also be expressed as the amount
necessary to provide a
single serving of concentrate.
[0017] The concentration factor of the liquid concentrate can be correlated
to one or more
of the ingredients in the liquid concentrate in reference to the desired level
of that ingredient in
the final beverage. By one approach, the concentration factor may be in terms
of the acidulant
content of the final beverage. For example, the concentration factor of the
liquid beverage
concentrate can be expressed as the level of dilution needed to obtain a final
beverage having an
acid range of about 0.01 to 1.0 percent by weight of the beverage, in another
aspect about 0.05 to
about 0.8 percent, and in yet another aspect about 0.1 to about 0.5 percent by
weight of the final
beverage. The amount of acid in a citrus-flavored beverage is generally
desired to be higher
than in other fruit-flavored beverages. Therefore, a final beverage having an
acid content of
about 0.1 to about 0.8 percent, in another aspect about 0.1 to about 0.5
percent, may be desired
for a citrus flavored beverage, while a final beverage having an acid content
of about 0.1 to
about 0.5, in another aspect about 0.1 to about 0.3 percent, may be desired
for a non-citrus, fruit-
flavored beverage.
[0018] By another approach, the concentration factor may in terms of the
sweetness of the
final beverage. For example, the concentration factor can be expressed as a
level of dilution
needed to provide a final beverage having a sweetness level equivalent to the
degree of
sweetness of a beverage containing about 5 to about 25 weight percent sucrose.
One degree Brix
corresponds to 1 gram of sucrose in 100 grams of aqueous solution. For
example, the dilution
factor of the beverage concentrate can be expressed as the dilution necessary
to provide an
equivalent of about 5 to about 25 degrees Brix, in another aspect about 8 to
about 14 degrees
Brix, and in another aspect about 8 to about 12 degrees Brix, in the resulting
beverage. By this
approach, one or more sweeteners can be included in the concentrated flavor
composition in an
amount effective to provide the beverage with a level of sweetness equivalent
to the desired
degrees Brix relative to sucrose.
[0019] The viscosity, pH, and formulations of the concentrates will depend,
at least in part,
on the intended dilution factor. In one approach, a moderately concentrated
product may be
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formulated to be diluted by a factor of at least 5 times to provide a final
beverage, which can be,
for example, an 8 ounce beverage. In one aspect, the concentrate is formulated
to be diluted by a
factor of about 5 to about 15 times to provide a final beverage. In this form,
the liquid
concentrate has a pH of about 1.8 to about 3.1, 1.8 to about 2.9, in another
aspect about 1.8 to
about 2.7, in another aspect about 1.8 to about 2.5, and in yet another aspect
about 1.8 to about
2.4, in another aspect about 2.0 to about 3.1, in another aspect about 2.0 to
about 2.9, in another
aspect about 2.0 to about 2.7, in another aspect about 2.0 to about 2.5, and
in yet another aspect
about 2.0 to about 2.4, and a viscosity of about 7.5 to about 100 cP, in
another aspect about 10 to
about 100 cP, in another aspect about 15 to about 100 cP, in another aspect
about 7.5 to about 50
cP, in another aspect about 10 to about 50 cP, in another aspect about 7.5 to
about 20cP, and in
another aspect about 10 to about 20 cP, as measured using Spindle SOO at 50
rpm at 20 C with a
Brookfield DVII + Pro Viscometer. Viscosity in the described range is
effective to increase the
stability of flavorings, colors, vitamins, and artificial sweeteners prone to
degradation at the
described pH. In one aspect, the concentrate includes at least about 0.1
percent acidulant, in
another aspect about 0.1 to about 15 percent acidulant, in another aspect
about 0.5 to about 10
percent acidulant, in another aspect about 0.75 to about 10 percent acidulant,
in another aspect
about 1 to about 10 percent acidulant, in another aspect about 0.75 to about 5
percent acidulant,
and in another aspect about 1 to about 5 percent acidulant by weight of the
concentrate.
[0020] In another approach, a highly concentrated product can be provided
at a
concentration of about 25 to about 200 times, in another aspect about 25 to
about 160 times, in
another aspect about 50 to about 160 times, in another aspect about 75 to
about 160 times, and in
yet another aspect about 75 to about 140 times that needed to provide a
desired level of flavor
intensity, acidity, and/or sweetness to a final beverage, which can be, for
example, an 8 ounce
beverage. In this form, the liquid concentrates described herein have a pH of
about 1.8 to about
3.1, 1.8 to about 2.9, in another aspect about 1.8 to about 2.7, in another
aspect about 1.8 to about
2.5, and in yet another aspect about 1.8 to about 2.4, in another aspect about
2.0 to about 3.1, in
another aspect about 2.0 to about 2.9, in another aspect about 2.0 to about
2.7, in another aspect
about 2.0 to about 2.5, and in yet another aspect about 2.0 to about 2.4, and
a viscosity for a
Newtonian liquid viscosity of about 7.5 to about 100 cP, in another aspect
about 10 to about 100
cP, in another aspect about 7.5 to about 50 cP, in another aspect about 10 to
about 50 cP, and in
another aspect about 7.5 to about 40 cP, in another aspect about 10 to about
40 cP. If the
8
concentrate instead has a non-Newtonian liquid viscosity, the viscosity may be
about 7.5 to
about 10,000 cP, in another aspect about 100 to about 10,000 cP, in another
aspect about 50 to
about 10,000 cP, in another aspect about 10 to about 10,000 cP, in another
aspect about 7.5 to
about 5,000 cP, in another aspect about 7.5 to about 1000 cP, in another
aspect about 7.5 to about
500 cP, in another aspect about 7.5 to about 200 cP, in another aspect about
7.5 to about 100 cP,
in another aspect about 7.5 to about 50 cP, and in another aspect about 7.5 to
about 40 cP.
Viscosity is measured using Spindle SOO at 10 rpm at 20 C with a Brookfield
DVII + Pro
Viscometer; however, if the machine registers an error message using Spindle
SOO for highly
viscous concentrates, Spindle S06 at 10 rpm at 20 C should be used. Viscosity
in the described
range is effective to increase the stability of flavorings, colors, vitamins,
and artificial sweeteners
prone to degradation at the described pH. In one aspect, the concentrate
includes at least about
0.5 percent acidulant, in another aspect about 0.5 to about 60 percent
acidulant, in another
aspect about 3 to about 35 percent acidulant, in another aspect about 8 to
about 35 percent
acidulant, in another aspect about 8 to about 30 percent acidulant, about 10
to about 30 percent
acidulant, and in yet another aspect about 15 to about 30 percent acidulant by
weight of the
concentrate. In another aspect, the concentrate has a concentration such that
when diluted with
a potable liquid at a ratio of about 1:50 to about 1:160 to provide a
beverage, the concentrate
delivers about 0.01 to 0.08 percent acid by weight of beverage.
[0021] Any edible, food grade organic or inorganic acid, such as, but not
limited to, citric
acid, malic acid, succinic acid, acetic acid, hydrochloric acid, adipic acid,
tartaric acid, fumaric
acid, phosphoric acid, lactic acid, sodium acid pyrophosphate, salts thereof,
and combinations
thereof can be used, if desired. The selection of the acidulant may depend, at
least in part, on
the desired pH of the concentrate and/or taste imparted by the acidulant to
the diluted final
beverage. In another aspect, the amount of acidulant included in the
concentrate may depend
on the strength of the acid. For example, a larger quantity of lactic acid
would be needed in the
concentrate to reduce the pH in the final beverage than a stronger acid, such
as phosphoric acid.
[0022] In some approaches, buffer can be added to the concentrate to
provide for increased
acid content at a desired pH. Use of buffer may be particularly desired for
more concentrated
products. Buffer can be added to the concentrate to adjust and/or maintain the
pH of the
concentrate. Depending on the amount of buffer used, a buffered concentrate
may contain
substantially more acid than a similar, non-buffered concentrate at the same
pH. In one aspect, buffer
may be included in an amount relative to the acidulant content. For example,
the acid:buffer ratio can
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be about 1:1 to about 25,000:1, in another aspect about 1.25:1 to about
4000:1, in another aspect about
1.7:1 to about 3000:1, and in another aspect about 2.3:1 to about 250:1. In
this respect, a buffered
concentrate may include more acidulant and can be diluted to provide a final
beverage with
enhanced tartness due to increased acidulant content as compared to a beverage
provided from
an otherwise identical concentrate at the same pH but which lacks buffers.
Inclusion of buffers
may also be advantageous to the flavor profile in the resulting final
beverage. In some aspects,
the concentrate may comprise about 0.5 to about 10.0 percent buffer.
[0023] Suitable buffers include, for example, a conjugated base of an acid,
gluconate,
acetate, phosphate or any salt of an acid (e.g., sodium citrate and potassium
citrate). In other
instances, an undissociated salt of the acid can buffer the concentrate.
[0024] The concentrate can be formulated to have Newtonian or non-Newtonian
flow
characteristics depending, at least in part, on the selection of viscosity
increasing agents. A
concentrate having Newtonian flow characteristics is characterized by a
viscosity independent
of the shear rate. Inclusion of certain viscosity increasing agents, for
example xanthan gum, can
create pseudo-plastic and shear thinning characteristics of the concentrate. A
drop in viscosity
as the shear rate increases indicates that shear thinning is occurring.
[0025] Increased viscosity can be achieved by the addition of one or more
viscosity
increasing agents in an amount effective to increase the viscosity of the
concentrate to the
desired level. For example, the viscosity increasing agent may be a nutritive
sweetener, polyol,
juice or juice concentrate, gum, gum derivative, cellulose derivative,
gelatin, polysaccharide,
carbohydrate, viscous solvent, starch, or combinations thereof. The amount of
the viscosity
increasing agent included in the concentrates described herein will depend, at
least in part, on
the amount necessary to achieve the desired viscosity.
[0026] Exemplary gums include, for instance, xanthan gum, guar gum, gum
arabic, tragacanth, gum
karaya, gum ghatti, locust bean gum, quince seed gum, and tamarind gum.
Exemplary polysaccharides
include, for instance, dextran, carrageenan, furcellaran, arabinogalactan,
alginate, pectin, and agar. Exemplary
cellulose derivatives include, for instance, carboxymethyl cellulose,
hydroxypropyl methylcellulose, and
microcrystalline cellulose. Exemplary carbohydrates include, for instance,
psyllium. Exemplary gum
derivatives include, for instance, propylene glycol alginate and low-methoxyl
pectin Starches derived from
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arrowroot, corn, potato, rice, sago, tapioca, waxy corn and wheat can also be
used to build up
viscosity.
[0027] Viscosity can also be increased by adding nutritive sweeteners such
as, for example,
honey, sucrose, fructose, glucose, tagatose, trehalose, galactose, rhamnose,
cyclodextrin (e.g., a-
cyclodextrin, 13-cyclodextrin, and y-cyclodextrin), maltodextrin (e.g.,
resistant maltodextrins
such as Fibersol-2Tm), dextran, ribulose, threose, arabinose, xylose, lyxose,
allose, altrose,
mannose, idose, lactose, maltose, invert sugar, isotrehalose, neotrehalose,
palatinose or
isomaltulose, erythrose, deoxyribose, gulose, idose, talose, erythrulose,
xylulose, psicose,
turanose, cellobiose, amylopectin, glucosamine, mannosamine, fucose,
glucuronic acid, gluconic
acid, glucono-lactone, abequose, galactosamine, beet oligosaccharides,
isomalto-
oligosaccharides (e.g., isomaltose, isomaltotriose, panose and the like), xylo-
oligosaccharides
(e.g., xylotriose, xylobiose and the like), gentio-oligoscaccharides (e.g.,
gentiobiose, gentiotriose,
gentiotetraose and the like), sorbose, nigero-oligosaccharides, palatinose
oligosaccharides,
fucose, fractooligosaccharides (e.g., kestose, nystose and the like),
maltotetraol, maltotriol,
malto-oligosaccharides (e.g., maltotriose, maltotetraose, maltopentaose,
maltohexaose,
maltoheptaose and the like), lactulose, melibiose, raffinose, rhamnose,
ribose, isomerized liquid
sugars such as high fructose corn or starch syrups (e.g., HFCS55, HFCS42, or
HFCS90), coupling
sugars, soybean oligosaccharides, glucose syrup, or combinations thereof.
[0028] Sweeteners included in the concentrates may include high intensity
sweeteners or
nutritive sweeteners, or a combination thereof, including, for example,
sucralose, aspartame,
saccharine, monatin, peptide-based high intensity sweeteners (e.g., Neotame0),
cyclamates
(such as sodium cyclamate), Luo Han Guo, acesulfame potassium, alitame,
saccharin,
neohesperidin dihydrochalcone, cyclamate, N41\143-(3-hydroxy-4-
methoxyphenyl)propy1]-L-a-
asparty1FL-10 phenylalanine 1-methyl ester, N4N43-(3-hydroxy-4-methoxypheny1)-
3-
methylbuty1FL-aaspartyll-L-phenylalanine 1-methyl ester, N4N43-(3-methoxy-4-
hydroxyphenyl)propyl]L-a-asparty1FL-phenylalanine 1-methyl ester, salts
thereof, stevia,
steviol glycosides, such as rebaudioside A (often referred to as "Reb A"),
rebaudioside B,
rebaudioside C, rebaudioside D, rebaudioside E, rebaudioside F, rebaudioside
A, rebaudioside
B, rebaudioside C, rebaudioside D, rebaudioside E, rebaudioside F, dulcoside
A, dulcoside B,
rubusoside, stevioside, and steviolbioside, and combinations thereof. The
selection of sweetener
and amount of sweetener added may depend, at least in part, on the desired
viscosity of the
11
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concentrated flavor composition and whether the sweetener is included as the
viscosity
increasing agent. For example, nutritive sweeteners like sucrose may be
included in much
higher amounts than high intensity sweeteners like neotame to provide the same
level of
sweetness and such higher total solids content contributed by the sweetener
increases the
viscosity of the composition. If desired, the sweetener can generally be added
in an amount of
about 0.2 to about 60 percent, with the lower end of the range generally more
appropriate for
high intensity sweeteners and the upper end of the range generally more
appropriate for
nutritive sweeteners. Other amounts of sweetener can also be included, if
desired.
[0029] Viscosity may also be increased through the use of one or more
polyol additives
such as, for example, erythritol, maltitol, mannitol, sorbitol, lactitol,
xylitol, inositol, isomalt,
propylene glycol, glycerol (glycerine), 1,3-propanediol, threitol, galactitol,
palatinose, reduced
isomalto-oligosaccharid es, reduced xylo-oligosaccharides, reduced gentio-
oligosaccharid es,
reduced maltose syrup, reduced glucose syrup, or combinations thereof.
[0030] The concentrates may also include one or more juices or juice
concentrates (such as
at least a 4x concentrated product) from fruits or vegetables for bulk solid
addition. In one
aspect, the juice or juice concentrate may include, for example, coconut juice
(also commonly
referred to as coconut water), apple, pear, grape, orange, potato, tangerine,
lemon, lime, tomato,
carrot, beet, asparagus, celery, kale, spinach, pumpkin, strawberry,
raspberry, banana,
blueberry, mango, passionfruit, peach, plum, papaya, and combinations. The
juice or juice
concentrates may also be added as a puree, if desired.
[0031] By another approach, replacement of at least some water of the
concentrate with a
solvent having a higher viscosity than water can also increase the viscosity
of the concentrate.
The viscosity and density of various solvents are provided in Table 1 below.
Beverage
concentrates where at least some of the water in the formulation has been
replaced with a
solvent having a higher viscosity and density than water will result in a more
viscous
concentrate than a comparative concentrate prepared without the higher
viscosity/density
solvent but with all other ingredients included at the same levels.
12
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Table 1. Approximate Physical Properties of Various Solvents at Room
Temperature
Liquid Viscosity (cP) Density (g/cc)
Water 1 1.00
Ethanol 1 0.79
1,3-Propanediol 52 1.06
Propylene Glycol 56 1.04
Glycerol 1200 1.26
Triacetin 25 1.16
[0032] It was found that the viscosity increasing agent does not have to
impact the amount
of bulk (free) solvent in the concentrate in order to be effective at
increasing the stability of the
ingredients. For example, it was found that xanthan gum does not impact the
amount of bulk
solvent in the concentrate but increases the viscosity while also increasing
stability of
ingredients prone to degradation. However, increased viscosity can be achieved
by inclusion of
water-binding ingredients, such as carbohydrates (e.g., sugar), fiber,
proteins, and
hydrocolloids, if desired. Inclusion of water-binding ingredients can
effectively slow the rate of
reactions by decreasing water activity and increasing viscosity. For example,
sugar effectively
binds bulk (free) solvent and causes the rate of diffusion to decrease by
increasing viscosity and
lowering water activity. It has been observed that this method can be used as
a means to slow
the rate of oxidation of flavors, including, for example, lemon oil. It was
found that a beverage
concentrate containing sugar slowed the rate of acid-catalyzed hydrolysis and
oxidation when
compared to a beverage free of sugar that was instead sweetened by a high-
potency sweetener.
Accordingly, reducing the amount of bulk solvent by adding water-binding
components to the
concentrate can slow the rate of diffusion-dependent reactions by increasing
viscosity and
lowering water activity. Advantageously, reduction of bulk water content also
results in
reduction in water activity, which can improve the microbial stability of the
concentrate.
[0033] The amount of water in the concentrate will generally be within
about 40 to about
98 percent. In one aspect, about 40 percent to about 90 percent water is
included. In another
aspect, about 40 percent to about 80 percent water is included.
[0034] The liquid concentrates described herein may include one or more
flavorings.
Generally about 0.5 to about 40 percent flavoring is included. Flavorings
useful in the liquid
concentrates described herein may include, for example, liquid flavorings
(including, for
13
example, alcohol-containing flavorings (e.g., flavorings containing ethanol,
propylene
glycol, 1,3-propanediol, glycerol, and combinations thereof), and flavor
emulsions (e.g.,
nano- and micro-emulsions)) and powdered flavorings (including, for example,
extruded,
spray-dried, agglomerated, freeze-dried, and encapsulated flavorings). The
flavorings may
also be in the form of an extract, such as a fruit extract. The flavorings can
be used alone or
in various combinations to provide the concentrate with a desired flavor
profile.
[0035] A
variety of commercially-available flavorings can be used, such as those sold
by Givaudan (Cincinnati, OH) and International Flavors & Fragrances Inc.
(Dayton, NJ). The
flavorings can be included at about 0.1 percent to about 40 percent, in
another aspect about
0.5 percent to about 40 percent, in another aspect about 1 percent to about 30
percent, and in
another aspect about 5 to about 20 percent by weight of the concentrates. In
some aspects,
the precise amount of flavoring included in the composition may vary, at least
in part, based
on the concentration factor of the concentrate, the concentration of flavor
key in the
flavoring, and desired flavor profile of a final beverage prepared with the
concentrate. In
some aspects, the flavouring includes a flavor key, and the acidulant and
flavor key are
provided in a ratio of about 1:2 to about 10,000:1. In some aspects, the
acidulant and flavor
key are provided in a ratio of about 1:1 to about 4000:1. Generally, extruded
and spray-dried
flavorings can be included in the concentrates in lesser amounts than alcohol-
containing
flavorings and flavor emulsions because the extruded and spray-dried
flavorings often
include a larger percentage of flavor key. Exemplary recipes for flavorings
are provided in
Table 2 below. Of course, flavorings with other formulations may also be used,
if desired.
14
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PCT/US2013/029844
Table 2: Exemplary Flavoring Formulations
Propylene Ethanol- Flavor Extruded Spray-
Dried
Glycol Containing Emulsions Flavorings
Flavorings
Flavorings Flavorings
Flavor key 1-20% 1-20% 1-10% 1-40% 1-40%
Water 0-10% 0-10% 70-80%
Ethanol 80-95%
Propylene 80-95% 0-4% 0-4%
glycol
Emulsifier 1-4% 0.1-10%
Carrier 1-95% 1-95%
Emulsion 15-20%
stabilizer
Preservative 0-2% 0-2% 0-2% 0-2% 0-2%
[0036] Many
flavorings include one or more non-aqueous liquids, typically in the form of
propylene glycol or ethanol. When such flavorings are included in the
concentrates described
herein, the non-aqueous liquid content of the flavorings is included in the
calculation of the
total NAL content of the concentrate. For example, if a flavoring has eighty
percent propylene
glycol and the flavoring is included in the concentrate at an amount of thirty
percent, the
flavoring contributes 24 percent propylene glycol to the total non-aqueous
liquid content of the
concentrate.
[0037]
Extruded and spray-dried flavorings often include a large percentage of flavor
key
and carrier, such as corn syrup solids, maltodextrin, gum arabic, starch, and
sugar solids.
Extruded flavorings can also include small amounts of alcohol and emulsifier,
if desired. Flavor
emulsions can also include carriers, such as, for example, starch. In one
aspect, the flavor
emulsion does not include alcohol. In other aspects, the flavor emulsion may
include low levels
of alcohol (e.g., propylene glycol, 1,3-propanediol, and ethanol). A variety
of emulsifiers can be
used, such as but not limited to sucrose acetate isobutyrate and lecithin, and
an emulsion
CA 02866266 2014-09-03
WO 2013/134627 PCT/US2013/029844
stabilizer may be included, such as but not limited to gum acacia. Micro-
emulsions often
include a higher concentration of flavor key and generally can be included in
lesser quantities
than other flavor emulsions.
[0038] In another aspect, a variety of different flavor emulsions may be
included in the
concentrated composition. Suitable flavor emulsions include, for example,
lemon, orange oil
lemonade, lemon oil lemonade, pink lemonade, floral lemonade, orange,
grapefruit, grapefruit
citrus punch, and lime from Givaudan (Cincinnati, OH). Of course, other flavor
emulsions or
types of emulsions, including nano- or micro-emulsions, may be used, if
desired.
[0039] In another aspect, a variety of different alcohol-containing
flavorings may be
included in the concentrated composition. The alcohols typically used in
commercially available
flavorings include compounds having one or more hydroxyl groups, including
ethanol and
propylene glycol, although others may be used, if desired. The flavoring may
also include 1,3-
propanediol, if desired. Suitable alcohol-containing flavorings include, for
example, lemon,
lime, cranberry, apple, watermelon, strawberry, pomegranate, berry, cherry,
peach,
passionfruit, mango, punch, white peach tea, sweet tea, and combinations
thereof. For example,
flavorings from commercial flavor houses include, for example, Lemon Lime,
Cranberry Apple,
Strawberry Watermelon, Pomegranate Berry, Peach Mango, White Peach Tea, and
Tea Sweet
from International Flavors & Fragrances Inc (New York, NY), as well as Peach
Passionfruit and
Tropical from Firmenich Inc. (Plainsboro, NJ). Other alcohol-containing
flavorings may be used,
if desired.
[0040] In yet another aspect, a variety of powdered flavorings may be
included in the
concentrate. The form of the powdered flavorings is not particularly limited
and can include,
for example, spray-dried, agglomerated, extruded, freeze-dried, and
encapsulated flavorings.
Suitable powdered flavorings include, for example, Natural & Artificial
Tropical Punch from
Givaudan (Cincinnati, OH), Natural & Artificial Orange from Symrise
(Teterboro, NJ), and
Natural Lemon from Firmenich Inc. (Plainsboro, NJ). Other powdered flavorings
may also be
used, if desired.
[0041] In some approaches, the acidulant and flavoring are included at a
ratio of at least
about 0.1:1, i.e., with "at least" meaning increasing quantities of acidulant
relative to flavoring,
16
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WO 2013/134627 PCT/US2013/029844
in another aspect at a ratio of at least about 0.5:1, in another aspect at a
ratio of at least about 1:1,
in another aspect at least about 1.5:1, and in yet another aspect at least
about 2:1.
[0042] If desired, the liquid beverage concentrates can further include
salts, preservatives,
viscosifiers, surfactants, stimulants, antioxidants, caffeine, electrolytes
(including salts),
nutrients (e.g., vitamins and minerals), stabilizers, gums, and the like.
Preservatives, such as
EDTA, sodium benzoate, potassium sorbate, sodium hexametaphosphate, nisin,
natamycin,
polylysine, and the like can be included, if desired, but are generally not
necessary for shelf
stability due to the low water content. Salts can be added to the concentrate
to provide
electrolytes, which is particularly desirable for sports-type or health
drinks. Exemplary salts
include, for example, sodium citrate, mono sodium phosphate, potassium
chloride, magnesium
chloride, sodium chloride, calcium chloride, the like, and combinations
thereof. For example,
sodium lactate, or other salts, may be used to provide a nutritive source of
minerals or for pH
buffering. By one approach, the additional ingredients can be included in any
combination and
in any amount so long as the desired pH and viscosity are achieved and
solubility of the
remaining ingredients is maintained. The amount of the additional ingredients
included may
also depend on the ability to solubilize or disperse the ingredients in the
concentrate.
[0043] Flavor Stability
[0044] The concentrates described herein provide enhanced flavor stability,
which is
particularly beneficial to very acid-labile ingredients. In some approaches,
"enhanced flavor
stability" and "avoiding substantial degradation of flavor" means that the
concentrates
described herein retain more flavor after storage at room temperature over the
shelf life of the
product as compared to an otherwise identical concentrate having a lower
viscosity due to a
difference in the amount of the viscosity increasing agent. In other
approaches, "enhanced
flavor stability" and "avoiding substantial degradation of flavor" means that
there is little
change in flavor and development of off flavor in the concentrate when stored
at 70 F in a
sealed container for at least about three months, in another aspect at least
about six months, and
in another aspect at least about nine months, and in yet another aspect at
least about twelve
months. If the ingredients are light sensitive, the container should be
impermeable to light. For
example, the change in flavor or development of off flavor notes can be
analyzed by a trained
flavor panel whereby the concentrate is diluted to provide a beverage and
compared to a
beverage prepared from an otherwise identical freshly prepared concentrate
(i.e., within 24
17
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WO 2013/134627 PCT/US2013/029844
hours and stored at room temperature in a sealed container) or concentrate .
By another
approach, the change in flavor or development of off flavor notes can be
analyzed by a trained
flavor panel whereby the concentrate is diluted to provide a beverage and
compared to a
beverage prepared from an identical concentrate, preferably from the same lot
or batch of
product, stored in a sealed container in the frozen state throughout its shelf
life and thawed at
room temperature immediately prior to testing. The concentrates can be
evaluated on a 10 point
scale, with a score of "1" being considered identical to control, "2-5" being
slightly/moderately
different than control, and "above 5" being unacceptably different from
control. A concentrate
achieving a score of 5 or less, in another aspect 4 or less, would be
considered to have acceptable
flavor stability. Analytical methods may also be used to determine if flavors
have oxidized or
otherwise deteriorated, including for example, gas chromatography, mass spec,
and HPLC.
[0045] Color and Vitamin Stability
[0046] The concentrates described herein provide enhanced stability to
color ingredients
and other ingredients where the degradation process includes browning (e.g.,
Vitamin C). As
used herein, "avoiding substantial degradation" of color and vitamin
ingredients is defined as a
change of less than about 5 percent, in another aspect less than about 10
percent, in another
aspect less than about 15 percent, and in another aspect less than about 20
percent, based on
changes in Ii'value of the Hunter Instruments L"ath color scale during storage
at 70 F in a
sealed container for at least about three months, in another aspect at least
about six months, and
in another aspect at least about nine months, and in yet another aspect at
least about twelve
months. If the ingredients are light sensitive, the container should be
impermeable to light. In
one exemplary method, the product after three months of storage at 70 F can be
compared to an
identical product, preferably from the same lot or batch of product, stored at
freezer
temperatures after manufacture and thawed at room temperature immediately
prior to testing.
[013471 The colors can include artificial colors, natural colors, or a
combination thereof and
can be included in the range of 0 to about 15 percent, in another aspect about
0.001 to 10
percent, in another aspect about 0.005 to 5 percent, and in yet another aspect
in the range of
about 0.005 to 1 percent, if desired. In formulations using natural colors, a
higher percent by
weight of the color may be needed to achieve desired color characteristics.
Exemplary colors
include natural beet juice powder, betalain, and annatto.
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[0048] It has been found that the stability of colors, particularly natural
colors, can be
enhanced in the increased viscosity formulations provided herein as compared
to an otherwise
similarly concentrated composition having a lower viscosity. The stability of
the color can be
quantified as measured on the Hunter Instruments L*a*b color scale. The L*a*b
scale describes
the color of a sample in terms of three color variables. The "L" scale
represents the tint of a
sample on a scale of 0 to 100, with a value of 100 representing white and a
value of zero
representing black. The "a" scale is a measure of the relative amount of green
or red light
reflected by the sample, with positive "a" values representing increasing
intensity of red and
negative "a" values representing increasing intensity of green. The "b" scale
is a measure of the
relative amount of blue or yellow light reflected by the sample, with positive
values
representing increasing intensity of yellow and negative values indicating
increasing intensity
of blue. The various types of colors generally degrade at different rates, but
the stability of a
particular color can be analyzed, for example, over a period of time at room
temperature in the
concentrates described herein in comparison to an otherwise identically
formulated concentrate
having lower viscosity.
[0049] The stability of Vitamin C can also be measured this way. As
described in more
detail later, Vitamin C (ascorbic acid) is known to degrade and brown when
solvated in an
acidic solution. Therefore, the onset of browning can be measured on the
Hunter Instruments
L*a*b color scale, particularly as indicated by a decrease in the L* value.
The stability of Vitamin
C can also be measured by titration, if desired.
[0050] Incorporation into Food and Beverages
[0051] The concentrates described herein can also be added to potable
liquids to form
flavored beverages. In some aspects, the concentrate may be non-potable (such
as due to the
high acid content and intensity of flavor). For example, the beverage
concentrate can be used to
provide flavor to water, cola, carbonated water, tea, coffee, seltzer, club
soda, the like, and can
also be used to enhance the flavor of juice. In one aspect, the beverage
concentrate can be used
to provide flavor to alcoholic beverages, including but not limited to
flavored champagne,
sparkling wine, wine spritzer, cocktail, martini, or the like.
[0052] The concentrates described herein can be combined with a variety of
food products
to add flavor to the food products. For example, the concentrates described
herein can be used
19
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to provide flavor to a variety of solid, semi-solid, and liquid food products,
including but not
limited to oatmeal, cereal, yogurt, strained yogurt, cottage cheese, cream
cheese, frosting, salad
dressing, sauce, and desserts such as ice cream, sherbet, sorbet, and Italian
ice. Appropriate
ratios of the beverage concentrate to food product or beverage can readily be
determined by one
of ordinary skill in the art.
[0053] Packaging
[0054] In one aspect, various quantities of the liquid beverage
concentrates may be
packaged in containers depending on the desired number of servings in the
container. For
example, more highly concentrated products may be packaged in smaller
quantities while still
delivering the same number of servings as a lesser concentrated product in a
larger package.
For example, a highly concentrated product could be packaged in the amount of
about 0.5 to
about 6 oz. of concentrate, in another aspect of about 1 to about 4 oz., and
in another aspect
about 1 to about 2 oz., with said quantity being sufficient to make at least
about 10 eight oz.
servings of flavored beverage. Lesser concentrated products could be packaged
in larger
amounts, such as about 10 to about 30 ounces to make at least about 10 eight
oz. servings of
flavored beverage. Of course, larger or smaller quantities may be packaged as
needed.
[0055] Advantages and embodiments of the liquid concentrate described
herein are further
illustrated by the following examples; however, the particular conditions,
processing schemes,
materials, and amounts thereof recited in these examples, as well as other
conditions and
details, should not be construed to unduly limit the compositions and methods
described
herein. All percentages in this application are by weight unless otherwise
indicated.
Examples
[0056] The following examples further illustrate various features of the
concentrates
described herein but are not intended to limit the scope as set forth in the
appended claims.
[0057] Example 1
[0058] This Example demonstrates the slowing of the rate of natural color
degradation via
an increase in viscosity through addition of gums that have little or no
effect on the volume of
bulk solvent in the composition. A control and experimental sample were
prepared according to
the formulations provided in Table 3 and then stored in a 70 F, light-free
environment.
CA 02866266 2014-09-03
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Table 3.
Control Sample Experimental Sample
(No Gums) (With Gums)
Water 65.14 63.86
Citric Acid 30.00 30.00
Red Beet Juice Powder 2.86 2.86
Potassium-Citrate 2.00 2.00
Xanthan Gum
0.00 1.28
(Ketrol-F [CP KELCO])
Total Weight 100.00 100.00
Water Activity (Aw) 0.948 0.940
4.74
Viscosity (cP) at 50rpm 4140
Viscosity (cP) at 100rpm 4.74 2400
[0059] The D'ath Values of each sample were tested at days 1, 4, 5, and 6
and compared to
each sample's D'a*b values at time zero. The percent change in the "a" value
and Delta-E Value
of the control sample was compared to the "a" value and Delta-E Value of the
experimental
sample. The results are provided in Table 4 below.
21
Table 4. L*a*b Values of Control and Experimental Samples on Days 0-6.
0
`µ)
Y Delta Descriptor -
dE dE CMC Metameris Yield of 41
--,
=.k
Product Storage Day L* a* b*
Transmission Rectangular
CMC (1 :c) m Index a*-Value i...)
r-
tV
Frozen 0 94.09 10.3 -3.95 85.48 N/A --.1
70 F 1 94.3 10.1 -4.13 85.97
Lighter, less red, bluer 0.28 2.00: 1.00 0.06 98.06%
Lighter, less red, less
70 F 4 96.18 6.53 -2.28 90.45
3.38 2.00: 1.00 0.85 63.40%
blue
Control
Lighter, less red, less
3.55
2.00: 1.00 0.89 61.46%
70 F 5 96.29 6.33 -2.2 90.72
blue
n
70 F 6 97.15 4.59 -0.83 92.8
Lighter, less red, less
5.39
2.00 : 1.00
blue
1.28 44.56% 0
1.)
OD
01
01
IV
C31
01
N
t=J
IV
Frozen 0 93.46 11.11 -4.09 84.02 N/A
o
1-
70 F 1 93.53 11.16 -4.55 84.19
Lighter, redder, bluer 0.46 2.00: 1.00 0.09 100.45% p.
I
2
I
Lighter, less red, less
3.03 2.00 : 1.00 0.77 68.59% 70 F
4 95.4 7.62 -2.58 88.56 o
blue
L,J
1.28%
Xanthan
Lighter, less red, less
2.88
2.00: 1.00 0.74 69.85%
70 F 5 95.34 7.76 -2.73 88.43
blue
Lighter, less red, less
4.44
2.00 : 1.00 1.07 56.53%
70 F 6 96.1 6.28 -1.42 90.25
blue
"0
n
c.)
t.J
=
-
=-o--
sz
oc,
.6.
.6.
CA 02866266 2014-09-03
WO 2013/134627 PCT/US2013/029844
[0060] It was found that after 6 days of storage, the "a" value of the
control sample
decreased from 10.3 to 4.59, whereas the "a" value of the experimental sample
decreased at a
slower rate from 11.11 to only 6.28.
[0061] The slower rate of color degradation in the experimental sample was
attributed to
the inclusion of xanthan gum and resulting increased viscosity of the
concentrate. It is not
believed that the slower rate of color degradation was due to changes in water
activity or the
amount of bulk solvent (i.e., the amount of solvent available for components
to diffuse
through).
[0062] Additionally, the L*a*b values of the control samples were compared
to those of the
experimental sample at each of days 1 to 6. The results are provided in Table
5 below.
23
Table 5. L*a*b Values and Pass/Fail of Control and Experimental Samples (1.28%
Xanthan) on Days 0-6.
Delta
dE 0
Y
dE Metameris t.)
Product Storage Day L* a* b*
Descriptor - CMC
Transmission
CMC m Index "C:4
Rectangular
(1 :c) _
1.28% Xanthan * 0 93.46 11.11 -4.09 84.02
r-
c.,
l,1
Control (No
Lighter, less 2.00 : --.1
* 0 94.09 10.3 -3.95 85.48
0.68 0.18
Xanthan) red,
less blue 1.00
1.28% Xanthan 70 F 1 93.53 11.16 -4.55 84.19
Control (No
Lighter, less 0.92 2.00 :
70 F 1 94.3 10.1 -4.13 85.97
0.24
Xanthan) red,
less blue 1.00
1.28% Xanthan 70 F 4 95.4 7.62 -2.58 88.56
Control (No
Lighter, less 2.00 :
70 F 4 96.18 6.53 -2.28 90.45
1.06 0.25 P
Xanthan) red,
less blue 1.00 0
Ni
1.28% Xanthan 70 F 5 95.34 7.76 -2.73 88.43
co
cn
0,
Control (No
Lighter, less 2.00: Ni
Xanthan)
t--)
r-
70 F 5 96.29 6.33 -2.2 90.72 .
141
red, less blue
1.00 0.33 cn
0,
Ni
1.28% Xanthan 70 F 6 96.1 6.28 -1.42 90.25
0
1-
p.
Control (No
Lighter, less 2.00 :
70 F 6 97.15 4.59 -0.83 92.8
181 04 0'
q:.
Xanthan) red,
less blue. .
1.00 1
0
L,J
-0
n
;=-1-
ci)
t.,
=
-
-i-
s.o
oc,
.6.
.6.
CA 02866266 2014-09-03
WO 2013/134627 PCT/US2013/029844
[0063] As shown in Table 5, there was no significant difference between the
initial (day 0)
and day 1 samples. More specifically, the delta-E values were less than 1 and
were 0.68 and 0.92,
respectively. On day 4, the difference between the control and experimental
samples was
significant. In particular, the delta-E value was 1.06. The significance of
the delta-E value
progressively increased and on days 5 and 6, the delta-E values were 1.41 and
1.81, respectively.
This indicates that on days 4, 5, and 6 that the 1.28% xanthan sample was
significantly different
visually than the control. A delta-E value greater than 1 indicates that the
optical difference
between two samples may be observed by the naked eye.
[0064] Overall, it was observed that, after day 1, the rate of degradation
of the control
sample was significantly higher than the rate of degradation of the
experimental sample. It was
also observed that although the initial rates of degradation of the control
sample and the
experimental sample were similar, the rate of degradation of the control
samples became
significantly faster over time compared to the rate of degradation of the
experimental sample.
[0065] Xanthan gum has a high polymer volume ratio (Rv) due to its high
molecular
weight and its low-degree of branching. The high Rv value of xanthan gum
enables it to "trap"
water that it is not chemically or physically bound to the xanthan gum,
meaning that the water
within the "spinning," solvated xanthan gum is free to bind to other chemicals
or molecules
within the "spinning" gum. Rv is the polymer volume ratio (Rv =
Vsphere/Vpolymer).
[0066] It was initially assumed that the "trapped" solution should have the
same degree of
diffusion within the effective volume as it would outside the effective
volume. It was found that
xanthan gum does not bind water and other solvated components directly and
increases the
viscosity without lowering the water activity. It was found that there was
essentially the same
amount of "bulk" (free) water with and without xanthan gum in the sample, and
xanthan gum
appeared to only bind whatever water it was directly associated with. This
caused a minimal
drop in the amount of "bulk" water in solution but caused a significant change
in the viscosity.
[0067] In terms of the red beet juice powder used as the natural colorant,
it was assumed
that the colorant should degrade at the same rate with or without xanthan gum
in solution. This
assumption was made due to the acid and the color freely diffusing inside of
the "trapped"
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volume. However, as discussed above, it was surprisingly found that the
xanthan gum slowed
the colorant's rate of degradation when compared to a sample free of xanthan
gum.
[0068] Example 2
[0069] In this Example, it was demonstrated that the rate of oxidation of
lemon flavor was
slowed by replacing a portion of the solvent (water) with more viscous
solvents that have little
or no effect on "bulk" solvent volume.
[0070] Lemon-
flavored beverage concentrates were prepared containing solvent systems of
(1) water, (2) water with ethanol, or (3) water with propylene glycol. The
rate of lemon flavor
oxidation and hydrolysis were observed by a sensory panel. The formulations of
the
concentrates are shown in Tables 6 and 7 below.
Table 6. Formulations of Concentrated Flavor Compositions Having Low Water
Content Using
Propylene Glycol
Ingredients 5% 10% Water 15% Water 25% Water 35% Water 64%
Water (Sample 2) (Sample 3) (Sample 4) (Sample 5) Water
(Sample 1) (Sample 6)
Water 5.0% 10.0% 15.0% 25.0% 35.0% 64.0175%
Propylene 59.0675% 54.0675% 49.0675% 39.0675% 29.0675%
0%
glycol
Citric acid 22.4% 22.4% 22.4% 22.4% 22.4% 22.4%
Potassium 0.6% 0.6% 0.6% 0.6% 0.6% 0.6%
citrate
Lemon 11.48% 11.48% 11.48% 11.48% 11.48% 11.48%
Sicilian
Generessence
Flavoring
(from IFF)
Sucralose 1.4204% 1.4204% 1.4204% 1.4204% 1.4204%
1.4204%
(dry)
EDTA 0.0321% 0.0321% 0.0321% 0.0321% 0.0321%
0.0321%
Potassium 0% 0% 0% 0% 0% 0.05%
sorbate
Total 100.0 100.0 100.0 100.0 100.0 100.0
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Table 7. Formulations of Concentrated Flavor Compositions Having Low Water
Content using
Ethanol.
High Water 5% Water 10% Water 15% Water 25% Water 35% Water
Comparative
Sample
Water 64.0175 5.0 10.0 15.0 25.0 35.0
Ethanol 0 58.3679 53.3679 48.3679 38.3679 28.3679
Citric acid 22.4 22.4 22.4 22.4 22.4 22.4
Potassium 0.6 0.6 0.6 0.6 0.6 0.6
citrate
Lemon 11.48 11.48 11.48 11.48 11.48 11.48
Sicilian
Generessence
Flavoring
(from IFF)
Sucralose 1.4204 1.4204 1.4204 1.4204 1.4204 1.4204
(dry)
EDTA 0.0321 0.0321 0.0321 0.0321 0.0321 0.0321
Potassium 0.05 0 0 0 0 0
sorbate
Total 100.0 100.0 100.0 100.0 100.0 100.0
[0071] It was found that solvent systems containing a mixture of
water/ethanol or
water/propylene glycol outperformed the single-solvent water systems in
slowing of the
degradation rate. The degree of outperformance was enhanced when the solvent
system
contained less water and more ethanol or propylene glycol. It was also found
that the water and
propylene glycol solvent system outperformed the water and ethanol systems,
especially as the
amount of water in these solvent systems was decreased and replaced by ethanol
or propylene
glycol.
[0072]
Accordingly, it appears that the addition of propylene glycol or ethanol into
the
beverage concentrate with decreased water content appears to cause a reduction
in the amount
of dissociated acid, which effectively reduces the amount of hydrogen ions
that can cause acid-
catalyzed flavor hydrolysis.
[0073] A secondary effect that was observed was how an increase in
viscosity decreases the
rate of acid-catalyzed hydrolysis and oxidation. Essentially the same amount
of bulk solvent
was present in all three systems. More specifically, whether the system
included water, ethanol,
or propylene glycol, there was approximately the same amount of unbound
solvent that
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beverage components could diffuse through. This secondary effect appeared to
outweigh the
impact of ethanol and propylene glycol limiting the dissociation of acid and
is discussed below
with reference to Table 8.
Table 8. pH and Viscosity for Low Water Lemon Concentrates in Ethanol and
Propylene Glycol
Water with Ethanol Water with Propylene Glycol
Water Viscosity Time to Failure Viscosity Time to Failure
pH pH
(cP)* stored at 90 F (cP) stored at 90 F
2.56 5.30 12-weeks 2.43 155.00 Passed for 12
weeks
2.64 7.20 10-weeks 2.33 114.00 Passed for 12
weeks
2.59 7.55 6-weeks 2.26 73.20 Passed for 12
weeks
2.41 7.68 4-weeks 2.12 37.40 6-weeks
2.20 7.74 4-weeks 1.94 20.00 6-weeks
63 1.71 4.03 2-weeks 1.76 4.54 2-weeks
*Viscosity read using a Brookfield DV-II + Pro viscometer, spindle #S00 @
500rpm.
100741 As can be seen in Table 8 above, the 5% water with ethanol sample
had a higher pH
than the 5% water with propylene glycol sample. If limiting the rate of
hydrolysis and oxidation
solely depended on acid dissociation, it would have been expected that the
ethanol sample
would have outperformed the propylene glycol sample. However, it was observed
that the 5%,
10%, and 15% water with propylene glycol samples had a longer shelf life than
the 5%, 10%,
and 15% water with ethanol samples. This outperformance appeared to be due to
the propylene
glycol samples having a significantly higher viscosity than the ethanol
samples. For example,
the 5% water with ethanol sample and the 5% water with propylene glycol sample
had
viscosities of 5.30 cP and 155.00 cP, respectively.
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[0075] Example 3
[0076] This Example demonstrates the slowing of acid-catalyzed flavor
hydrolysis and
oxidation through the addition of water-binding components that lower water
activity (amount
of "bulk" solvent) and increase viscosity.
[0077] Two 7X beverage concentrates were made according to the recipes of
Table 9 below:
(1) a control including, in pertinent part, lemon flavor, sucralose, but no
sucrose; and (2) an
experimental sample including, in pertinent part, lemon flavor and sucrose
(but no sucralose).
Table 9. Liquid Beverage Concentrate Formulations
Experimental Control
(High Viscosity, (Low Viscosity,
Low Water High Water
Activity) Activity)
(% by wt) (% by wt)
Water 51.07920 96.5596
Sucrose 45.15 0
Potassium Sorbate 0.05 0.05
Potassium citrate 0 0.25
Sodium citrate 0.20000 0
Givaudan Natural Lemon Flavor Emulsion 1.2 1.2
Sucralose Liquid 0 0.5
Yellow#5 0.0008 0.0004
Citric Acid 2.25000 1.425
Sodium benzoate 0.05 0
Sodium metabisulfite 0.005 0
Rosemary Extract 0.015 0.015
Total Sum: 100 100
Viscosity (@ 20 C) [Spindle #S00, 20 rpm] 16.6 cP 3.46 cP
Water Activity 0.895 0.995
pH 2.46 2.70
[0078] It was observed that the control sample, which had lower viscosity
and higher
water activity, oxidized to an unacceptable level after being stored at 90 F
for 4 weeks.
Conversely, the experimental sample, which had higher viscosity and lower
water activity, did
not oxidize to a level that was considered unacceptable after 12 weeks of
storage at 90 F. Also, it
should be noted that the experimental sample had a higher acid concentration
and lower pH
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versus the control sample which would have been expected to increase the rate
of degradation.
Each sample was subsequently used to provide a beverage by diluting 1 part
concentrate in 6
parts water.
[0079] While the experimental sample had both a lower water activity and
higher viscosity
when compared to the control, the reduction in water activity was not believed
to be significant
enough to cause a decreased rate of oxidation. It is known by those skilled in
the art that rates of
chemical reactions such as lipid oxidation and non-enzymatic browning are not
significantly
reduced at a water activity around 0.895 or higher. It is known that the rate
of chemical
reactions do not significantly slow until water activity is reduced below
approximately 0.7.
Therefore, it appears that the increase in viscosity, and not decreased water
activity, due to
addition of sucrose resulted in the decreased rate of lemon flavor oxidation.
[0080] Example 4
[0081] This example demonstrates the rate of (1) Vitamin C degradation and
(2) browning
due to Vitamin C can be slowed through an increase in viscosity of the
solution solvating the
Vitamin C. The increase in viscosity was attained via an addition of gums or
an addition of a
bulk sweetener such as glucose. All samples in this example were prepared at
70 F via simple
agitation and then stored at 70 F in a light-free environment.
[0082] Vitamin C (ascorbic acid) is known to degrade and brown when
solvated in an
acidic solution. It is believed that early breakdown products of Vitamin C
still have
functionality. Unlike other vitamins used to fortify beverages, Vitamin C can
brown the
beverage while not losing all functionality. Therefore, assessing the browning
of Vitamin C
appears to be a suitable way to evaluate Vitamin C functionality during the
shelf-life of the
beverage.
[0083] Part A:
[0084] In the first part of the experiment, samples were prepared according
to Table 10
below which lack Vitamin C to show that little to no browning occurs in the
absence of Vitamin
C. The samples were prepared at 70 F via simple agitation and then stored at
70 F in a light-free
environment. Viscosity was measured at 10 rpm at 20 C using spindle #500 with
a Brookfield
viscometer.
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Table 10: Composition of Control and Variant Samples.
Vitamin C Vitamin C
Vitamin C Free
Free with Free with
Control
0.08% Xanthan 0.32% Xan than
(%/wt.)
(%/wt.) (%/wt.)
Water 70.14 70.06 69.82
Xanthan Gum 0.00 0.08 0.32
Citric Acid 16.50 16.50 16.50
Malic Acid 4.12 4.12 4.12
Potassium
1.50 1.50 1.50
Citrate
Acesulfame
0.84 0.84 0.84
Potassium
Sucralose 25%
6.85 6.85 6.85
Solution
Potassium Sorbate 0.05 0.05 0.05
Total Sum: 100 100 100
pH 2.12 2.11 2.13
Viscosity (cP) 4 35 200
100851 After 8
months of storage, the 1_,*ath values of the three samples were measured.
Based on the Va*b values of the Table 11, it was found that the long-term
solvation of xanthan
gum, citric acid, sucralose, malic acid, acesulfame potassium and potassium
sorbate in Water at
most caused an insignificant amount of browning.
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Table 11: L*a*b values of Composition of Control and Variant Samples after 8
months of storage
in a 70F, light-free environment.
Months
Sample Storage L* a* b*
at 70 F Transmission
Vitamin C Free Control 8 99.84 -0.25 1.46 99.59
Vitamin C Free with 0.08%
8 100.03 -0.18 0.76 100.07
Xanthan
Vitamin C Free with 0.32%
8 99.6 -0.21 1.22 98.96
Xanthan
[0086] Part B:
[0087] In the second part of the experiment, samples were prepared that
include Vitamin C
according to Table 12 below. Viscosity was measured using a Brookfield DV-II +
Pro viscometer
using spindle #500 at 10 rpm and 50 rpm. The pH and viscosity measurements
were
performed on the undiluted, concentrated samples at 20 C.
32
Table 12: Composition of Control and Variant Samples
Variant 2
Variant 4 Variant Variant 6 o
Control Variant 1 Variant 3
t.)
(0.08% (0.32% 5 (20% =
Control with (0.08% (0.32%
41
Xanthan
Xanthan (20% Glucose ,
EDTA Xanthan) Xanthan)
.
with EDTA)
with EDTA) Glucose) with EDTA) ca
r-
c.,
l,1
Water 68.33% 68.33% 68.25% 68.25% 68.01%
68.01% 48.33% 48.33% --.1
Citric Acid 16.48% 16.48% 16.48% 16.48% 16.48%
16.48% 16.48% 16.48%
Potassium
0.05% 0.05% 0.05% 0.05% 0.05% 0.05% 0.05%
0.05%
Sorbate
Potassium
1.50% 1.50% 1.50% 1.50% 1.50% 1.50% 1.50%
1.50%
Citrate
Sucralose
0
1.)
co
25% 6.85% 6.85% 6.85% 6.85% 6.85%
6.85% 6.85% 6.85% cn
0,
1.)
Solution
cn
w
0,
(.4
Malic Acid 4.12% 4.12% 4.12% 4.12% 4.12%
4.12% 4.12% 4.12% I.)
0
1-
p.
1 Acesulfame
0.84% 0.84% 0.84% 0.84% 0.84% 0.84% 0.84%
0.84% 0
q)
1 Potassium
0
Vitamin C 1.83% 1.83% 1.83% 1.83% 1.83%
1.83% 1.83% 1.83% L,4
Glucose 0% 0% 0% 0% 0%
0% 20.0% 20.0%
Xanthan
0% 0% 0.08% 0.08% 0.32% 0.32% 0%
0%
Gum
EDTA 0.0000% 0.0025% 0% 0.0025% 0% 0.0025% 0%
0.0025%
-o
Total Sum: 100.00 100.00 100.00 100.00 100.00
100.00 100.00 100.00 n
;=-1-
u)
pH 2.12 2.13 2.12
2.12 t.4
=
Viscosity (cP)
w
4 35 200 14
-i-
at 10 rpm
sz
oo
Viscosity (cP)
.6.
.6.
4 21 100 14
at 50 rpm
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[0088] The percent of Vitamin C remaining in the control and experimental
samples was
measured at 0, 4, 8, and 11 weeks after storage at 70 F in a light free
environment. Samples were
diluted with water to an expected level of 150 ppm Vitamin C prior to
measurement. The results
are presented in Table 13 below.
Table 13: Percent of Vitamin C Remaining After Storage
Variant Variant
Control Variant 3
1 5
Time Zero 100.07% 100.00% 99.60% 100.53%
Week 4 93.32% 98.65% 97.59% 97.32%
Week 8 83.46% 93.99% 89.32% 91.19%
Week 11 82.66% 89.32% 86.66% 85.32%
[0089] It was found that the addition of xanthan gum or glucose slowed the
rate of Vitamin
C deterioration through 11 weeks of storage. It was found that after 11 weeks
of storage the
Control sample had an approximate yield of 83% compared to yields of 89%, 87%,
and 85% in
Variant 1(0.08% Xanthan), Variant 3 (0.32% xanthan), and Variant 5 (20%
Glucose), respectively.
[0090] Thus, the inclusion of xanthan gum or glucose in the experimental
samples
appeared to slow the rate of Vitamin C deterioration as a result in the change
of viscosity. As
can be seen in Table 12 above, the inclusion of xanthan gum or glucose did not
impact the pH of
any samples.
[0091] Additionally, the L"ath values of the control and experimental
samples (in
undiluted concentrate form) are provided in Table 14 below.
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Table 14: L"a*b values of Control and Experimental samples after 0, 4, 5, 6,
7, 9, and 11 weeks of
storage.
Weeks Y
Sample Storage L* a* b*
at 70 F Transmission
0 99.22 -0.08 0.53 98
4 95.78 -5.11 30.95 89.47
92.92 -3.57 46.92 82.78
Control 6 89.78 -0.46 56.74 75.83
7 85.88 4.61 68.1 67.75
9 76.21 17.37 85.49 50.23
11 68.14 27 92.23 38.16
4 99.13 -2.61 9.73 97.78
5 97.94 -3.47 17.04 94.77
Control
with EDTA 6 96.73 -3.64 23.14 91.77
7 94.67 -2.97 32.77 86.83
11 81.58 9.84 70.28 59.52
0 99.02 -0.04 0.66 97.5
4 97.96 -3.72 15.57 94.81
5 95.84 -4.52 30.33 89.62
Variant-
6 93.78 -3.63 39.36 84.77
0.08% Xanthan
7 90.64 -0.81 50.81 77.7
9 82.48 8.77 72.01 61.19
11 75.14 17.82 83.2 48.5
4 99.37 -1.69 6.03 98.38
Variant- 5 98.76 -2.35 10.24 96.83
0.08% Xanthan and 6 97.8 -2.83 15.13 94.41
EDTA 7 96.59 -2.82 21.56 91.44
11 87.65 3.33 52 71.34
0 99.28 -0.09 0.77 98.14
4 96.64 -3.83 18.1 91.55
Variant- 5 94.97 -4.09 27.79 87.54
0.32% Xanthan 6 93.35 -3.63 35.95 83.76
7 90.46 -1.32 47.33 77.31
9 83.4 6.91 67.78 62.92
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11 76.39 15.68 80.03 50.52
4 97.72 -2.01 8.57 94.21
Variant- 5 97.06 -2.52 13.18 92.58
0.32% Xanthan and 6 96.15 -2.83 18.1 90.38
EDTA 7 94.71 -2.62 25.14 86.94
11 85.88 4.47 54.8 .. 67.75
0 100.1 -0.05 0.32 100.29
4 98.9 -3.02 11.99 97.18
5 97.59 -3.76 20.59 .. 93.91
Variant -
6 96.08 -3.55 27.49 90.19
20% Glucose
7 93.82 -2.29 36.98 84.85
9 87.57 3.52 56.31 71.17
11 80.95 10.9 70.03 58.39
4 99.37 -1.95 7.41 98.37
Variant- 5 98.57 -2.48 12.29 96.34
20% Glucose and 6 97.67 -2.77 17.33 94.09
EDTA 7 96.15 -2.5 24.71
90.36
11 86.52 5.02 56.42 69.03
[0092] It was found that the addition of xanthan gum or glucose slowed the
rate of
browning from Vitamin C through 11 weeks of storage. From the L*a*b values
listed in Table 11
above, it is known that the long-term solvation of xanthan gum, citric acid,
sucralose, malic
acid, acesulfame potassium and potassium sorbate in water at most caused an
insignificant
amount of browning, leaving Vitamin C as the most probable cause of browning.
[0093] After 11 weeks of storage, the L*a*b values for the control were
68.14, 27, and 92.23,
respectively after their initial values of 99.22. -0.08, and 0.53,
respectively, at time zero. It was
found, after 11 weeks of storage, the L*a*b values for the Variant 1 (0.08%
xanthan) were 75.14,
17.82, and 83.2 respectively after their initial values of 99.02. -0.04, and
0.66, respectively, at time
zero. The differences in the L*a*b values between the control and Variant 1
were 7.00, 9.18, and
9.03, respectively, which correspond to Variant 1 being clearer, less yellow,
and less red than the
control.
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[0094] After 11 weeks of storage, the differences in the L*a*b values
between the control
and Variant 3 (0.32% xanthan) were 8.25, 11.32, and 12.20, respectively, which
correspond to
Variant 3 being clearer, less yellow, and less red than the control.
[0095] After 11 weeks of storage, the differences in the L*a*b values
between the control
and Variant 5 (20% Glucose) were 12.81, 16.10, and 22.20, respectively, which
correspond to
Variant 5 being clearer, less yellow, and less red than the control.
[0096] After 11 weeks of storage, the L*a*b values for Variant 2 (0.08%
xanthan with
EDTA) were 87.65, 3.33, and 52, respectively. The difference in the L*a*b
values between the
control with EDTA and Variant 2 were 6.07, 6.51, and 18.28, respectively,
which correspond to
Variant 2 being clearer, less yellow, and less red than the control with EDTA.
[0097] After 11 weeks of storage, the difference in the L*a*b values
between the control
with EDTA and Variant 4 (0.32% xanthan with EDTA) were 4.30, 5.37, and 15.48,
respectively,
which correspond to Variant 4 being clearer, less yellow, and less red than
the control with
EDTA.
[0098] After 11 weeks of storage, the difference in the L*a*b values
between the control
with EDTA and Variant 6 (20% Glucose with EDTA) were 4.94, 4.82, and 13.86,
respectively,
which correspond to Variant 6 being clearer, less yellow, and less red than
the control with
EDTA.
[0099] The L*a*b values of Variants 1-6 demonstrate that the Variant
samples had
undergone less browning than the controls. Thus, the inclusion of xanthan gum
or glucose in
the experimental samples appeared to slow the rate of browning from Vitamin C
as a result in
the change of viscosity. The inclusion of EDTA was not necessary for xanthan
gum or glucose to
slow the rate of browning from Vitamin C but a coupling effect was observed.
EDTA, glucose,
or xanthan gum each individually were effective at slowing the rate of
browning, but the
inclusion of EDTA with xanthan gum or glucose were able to more significantly
slow the rate of
browning.
[00100] Example 5
[00101] This example demonstrates slowing the rate of flavor deterioration
and oxidation
through the addition of water-binding components (coconut water concentrate)
that increase
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the viscosity of the beverage concentrate solution. Coconut water is extracted
from coconuts
and can be further concentrated through the removal of water and possibly the
removal of fiber.
Coconut water is not extracted from the meat of the coconut (this would be
referred to as
coconut cream). Coconut water is the free-standing, unbound water inside a
coconut. This
ingredient can be purchased through multiple juice suppliers.
[00102] Two 90X beverage concentrates were made according to the
formulations in Table
15 below. Viscosity was measured using a Brookfield DV-11 + Pro viscometer
using spindle
#S00 at 10 rpm. The pH and viscosity measurements were performed on the
undiluted,
concentrated samples at 20 C. The beverage concentrates were stored at 70 F
and 90 F.
Table 15: Composition of Control and Experimental Samples with pH and
viscosity
Experimental
Control Sample
Sample
% Weight % Weight
Water 72.99 39.24
60 Brix
Coconut Water Concentrate
0.00 33.75
Acidified with Citric Acid (pH 3.8 to about
4.2)
Malic Acid 13.50 13.50
Sucralose Solution (25%) 5.57 5.57
Tropical Punch Flavor (Propylene Glycol
4.13 4.13
Based)
Citric Acid 1.58 1.58
Potassium Citrate 1.35 1.35
Yellow 5 0.08 0.08
Red 40 0.07 0.07
Acesulfame Potassium 0.69 0.69
Potassium Sorbate 0.05 0.05
Total Sum 100 100
Viscosity (cP) 10.5 2
pH 2.54 2.53
[00103] The concentrates were diluted (1 part concentrate to 89 parts
water) to prepare
beverages before the beverages were analyzed by a team of panelists. Tastings
were performed
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at weeks 6, 8, 10, and 12 for the samples stored at 70 F and 90 F. In
addition, for the samples
stored at 70 F, tastings were also performed at months 5, 7, and 9. A minimum
of 5 panelists
compared the degree of difference of flavor oxidation and deterioration. The
samples were
tasted blind and the degree of difference of the control and experimental
sample was compared
to their own sample, frozen at time zero and thawed prior to tasting. The
scale for degree of
difference was as followed: 1 = no difference; 2 to 5 = acceptable difference;
and 6 to 10 =
unacceptable difference. The results are presented below in Table 16.
[00104] It was observed that after 12 weeks of storage at 90 F and 9 months
of storage at
70 F, less flavor deterioration and oxidation occurred in the experimental
sample containing
coconut water concentrate.
Table 16: Degree of Difference of Control and Experimental Sample through 9
Months of
Storage at 70 F and 12 Weeks of storage at 90 F
Difference
Storage Storage Experimental
Control Between
Time Temperature Sample
Samples
70 F 4.1 2.8 1.3
Week 6
90 F 3.4 3 0.4
70 F 3.3 3.2 0.1
Week 8
90 F 4.2 3.4 0.8
70 F 4.5 3.8 0.7
Week 10
90 F 3.1 2.9 0.2
70 F 3.9 2.1 1.8
Week 12
90 F 4.5 3.8 0.7
Month 5 70 F 3.9 2.9 1
Month 7 70 F 4.5 2.1 2.4
Month 9 70 F 5 2.9 2.1
[00105] As demonstrated in the table above, the inclusion of coconut water
concentrate in
the experimental sample appeared to slow the rate of flavor deterioration and
oxidation as a
result in the change of viscosity.
[00106] Example 6
[00107] This example demonstrates how xanthan Gum and fructose impact
viscosity when
added to a beverage concentrate at different use levels. Viscosity was
measured across multiple
39
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WO 2013/134627 PCT/US2013/029844
spindle speeds to differentiate non-Newtonian and Newtonian solutions from one
another.
Samples were prepared according to the formulations of Table 17 below. The
viscosities and pH
of the samples were measured using a Brookfield DV-H + Pro viscometer (Table
18). The pH
and viscosity measurements were performed on the undiluted, concentrated
samples at 20 C.
Table 17: Compositions of Control and Experimental Samples of 120X beverage
concentrates.
Experimental Samples
0.08% 0.16% 0.32% 0.64% 1.28% 10%
20% 30%
Control Xanthan Xanthan Xanthan Xanthan Xanthan Fructose Fructose Fructose
Water 70.14% 70.06% 69.98% 69.82% 69.50% 68.86%
60.14% 50.14% 40.14%
Xanthan Gum 0% 0.08% 0.16% 0.32% 0.64% 1.28% 0%
0% 0%
Fructose 0% 0% 0% 0% 0% 0% 10.0%
20.0% 30.0%
Citric Acid 16.50% 16.50% 16.50% 16.50% 16.50% 16.50%
16.50% 16.50% 16.50%
Malic Acid 4.12% 4.12% 4.12% 4.12% 4.12% 4.12% 4.12%
4.12% 4.12%
Potassium
1.50% 1.50% 1.50% 1.50% 1.50% 1.50% 1.50% 1.50% 1.50%
Citrate
Acesulfame
0.84% 0.84% 0.84% 0.84% 0.84% 0.84% 0.84% 0.84% 0.84%
0
1.)
Potassium
co
Sucralose 25%
1.)
6.85% 6.85% 6.85% 6.85% 6.85% 6.85% 6.85% 6.85% 6.85%
Solution
NJ
Potassium
0
0.05% 0.05% 0.05% 0.05% 0.05% 0.05% 0.05% 0.05% 0.05%
Sorbate
0
Total Sum: 100.0 100.0 100.0 100.0 100.0 100.0 100.0
100.0 100.0
0
-0
;=-1-
ci)
CA 02866266 2014-09-03
WO 2013/134627 PCT/US2013/029844
Table 18: Viscosities of Control and Experimental Samples
Spindle
Sample 10 RPM 20 RPM 50 RPM 100 RPM pH
Type
Control SOD 4 4 4 4 2.12
with 0.08%
SOD 35 30 21 17 2.11
Xanthan Gum
with 0.16%
SOD 72 55 38 29 2.13
Xanthan Gum
with 0.32%
SOD 208 160 100 Error 2.12
Xanthan Gum
with 0.64%
S06 3600 2200 1180 730 2.13
Xanthan Gum
with 1.28%
S06 4300 2500 1300 800 2.12
Xanthan Gum
with 10%
SOD 7 7 7 - 2.13
Fructose
with 20%
SOD 14 14 14 - 2.11
Fructose
with 30%
SOD 39 39 39 - 2.12
Fructose
[00108] Thus, the inclusion of fructose or xanthan in the beverage
concentrate increased the
viscosity of the solution.
[00109] The foregoing descriptions are not intended to represent the only
forms of the
concentrate and methods in regard to the details of formulation. The
percentages provided
herein are by weight unless stated otherwise. Changes in form and in
proportion of parts, as
well as the substitution of equivalents, are contemplated as circumstances may
suggest or
render expedient. Similarly, while concentrates and methods have been
described herein in
conjunction with specific embodiments, many alternatives, modifications, and
variations will be
apparent to those skilled in the art in light of the foregoing description.
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