U.S. patent application number 12/167301 was filed with the patent office on 2008-10-30 for compositions containing green tea catechins and one or more polyvalent mineral cations.
This patent application is currently assigned to The Procter & Gamble Company. Invention is credited to Jeffrey John Kester, Ashok Premchand Luhadiya, Gerhard Norbert Zehentbauer.
Application Number | 20080268129 12/167301 |
Document ID | / |
Family ID | 34079072 |
Filed Date | 2008-10-30 |
United States Patent
Application |
20080268129 |
Kind Code |
A1 |
Kester; Jeffrey John ; et
al. |
October 30, 2008 |
COMPOSITIONS CONTAINING GREEN TEA CATECHINS AND ONE OR MORE
POLYVALENT MINERAL CATIONS
Abstract
Disclosed are beverage compositions containing green tea
catechins and polyvalent mineral cations, wherein the beverage
compositions exhibit a relatively low turbidity. Also disclosed is
a process for avoiding the turbidity issues associated with
inclusion of calcium and green tea catechins.
Inventors: |
Kester; Jeffrey John; (West
Chester, OH) ; Luhadiya; Ashok Premchand;
(Cincinnati, OH) ; Zehentbauer; Gerhard Norbert;
(Okeana, OH) |
Correspondence
Address: |
THE PROCTER & GAMBLE COMPANY;Global Legal Department - IP
Sycamore Building - 4th Floor, 299 East Sixth Street
CINCINNATI
OH
45202
US
|
Assignee: |
The Procter & Gamble
Company
|
Family ID: |
34079072 |
Appl. No.: |
12/167301 |
Filed: |
July 3, 2008 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
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10883446 |
Jul 1, 2004 |
7419693 |
|
|
12167301 |
|
|
|
|
60484790 |
Jul 3, 2003 |
|
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Current U.S.
Class: |
426/597 |
Current CPC
Class: |
A23F 3/18 20130101; A23F
3/14 20130101; A23F 3/20 20130101; A23V 2002/00 20130101; A23V
2200/308 20130101; A23V 2250/214 20130101; A23V 2250/1578 20130101;
A23V 2200/326 20130101; A23V 2200/33 20130101; A23F 3/163 20130101;
A23V 2002/00 20130101 |
Class at
Publication: |
426/597 |
International
Class: |
A23F 3/16 20060101
A23F003/16 |
Claims
1. A process for treating a tea extract, the process comprising:
(a) providing a tea extract in a liquid form, (b) combining the tea
extract and a soluble calcium source, (c) permitting the tea
extract and soluble calcium source to interact under conditions
sufficient to form a precipitate of insoluble calcium components,
and (d) separating the insoluble calcium components from the tea
extract.
2. The process according to claim 1, wherein the soluble calcium
source is added to the tea extract at a concentration from about
400 mg to about 10,000 mg per 100 gm of tea extract on a dry weight
basis.
3. The process according to claim 1, wherein the soluble calcium
source is selected from the group consisting of calcium sulfate,
calcium chloride, calcium acetate, calcium gluconate, or mixtures
thereof.
4. The process according to claim 3, wherein the insoluble calcium
components in tea extract on a dry weight basis is not present in
more than about 1% by weight.
5. The process according to claim 3, wherein the insoluble calcium
components in the tea extract on a dry weight basis is not present
in more than 0.6% by weight.
6. The process according to claim 1, wherein the insoluble calcium
components in the tea extract on a dry weight basis is not present
in more than 0.1% by weight.
7. The process according to claim 1, wherein the tea extract at
step (a) comprises at least 10% green tea catechins on a dry weight
basis.
8. The process according to claim 1, wherein the tea extract at
step (a) comprises at least 20% green tea catechins on a dry weight
basis.
9. The process according to claim 1, wherein treatment conditions
at step (a) are carried out at ambient temperatures.
10. The process according to claim 1, wherein treatment conditions
at step (c) are carried out at high temperatures.
11. The process according to claim 1, wherein treatment is greater
than about 130 degrees F.
12. The process according to claim 1, wherein treatment is greater
than about 145 degrees F.
13. The process according to claim 1, wherein treatment is greater
than about 160 degrees F.
14. The process according to claim 1, wherein treatment conditions
at step (c) are carried at a reaction time of 2 hours or less.
15. The process according to claim 1, wherein treatment conditions
at step (c) are carried at a reaction time of 45 minutes or
less.
16. The process according to claim 1, wherein treatment conditions
at step (c) are carried at a reaction time of 15 minutes or
less.
17. The process according to claim 1, further comprising: (e)
addition of acid.
18. The process according to claim 17, wherein the acid is a
food-grade acid.
Description
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a divisional of U.S. application Ser.
No. 10/883,446, filed Jul. 1, 2004, which claims the benefit of
priority to U.S. Provisional Application Ser. No. 60/484,790, filed
Jul. 3, 2003, which are herein incorporated by reference.
FIELD OF INVENTION
[0002] The present invention relates to compositions containing
green tea catechins and one or more polyvalent mineral cations.
Such compositions include ready-to-drink (RTD) beverages, as well
as powders and concentrates that are combined with an aqueous
liquid to form a consumable beverage.
BACKGROUND
[0003] Consumption of tea, particularly green tea, has increasingly
been associated with therapeutic benefits in the areas of
cardiovascular health and cancer prevention. These and other health
benefits have been attributed to the unoxidized flavanols in green
tea, i.e. the catechin monomers. As a result of these health
benefits, there has been a substantial increase in the number of
entrants of tea containing beverages into the ready-to-drink
beverage market. Currently, many tea containing beverages are sold
in the form of bottled, canned or carton-boxed products. Many of
the beverages contain black tea extract with fruit juice, fruit
aroma or fruit flavors, while others contain only tea flavors. When
black tea is used in beverages, many of the published health
benefits of the unoxidized flavanols (green tea catechins) are not
realized by the consumer because black tea contains oxidized,
polymerized flavanols. While certain beverage products contain
green tea extract, these beverages generally contain a relatively
low level of the beneficial catechins and typically do not contain
a significant level of polyvalent mineral cations. The beverages
also typically have a brown color or contain natural or artificial
colorants to mask the brown color, or the beverages have a turbid
appearance. There are not any green tea-containing beverages
currently on the market that possess the combination of a
relatively high level of catechins, one or more polyvalent mineral
cations, and a relatively high degree of clarity (i.e. low
turbidity). Therefore, there is a need for such green
tea-containing beverages.
[0004] It is an object of this invention to provide compositions
that contain significant levels of green tea catechins and one or
more polyvalent mineral cations, wherein such compositions, when
prepared in a final beverage form, are relatively clear. In one
particular embodiment, the final beverage has a low level of brown
color such that the appearance of the beverage is not typical of
tea, but rather is similar to water.
SUMMARY OF THE INVENTION
[0005] In one aspect, the present invention relates to a fortified
ready-to-drink (RTD) beverage composition comprising (1) at least
about 100 ppm green tea catechins; and (2) at least about 10% of
the U.S. Reference Daily Intake (RDI) of one or more polyvalent
mineral cations per 250 mL of the composition; wherein the
composition exhibits a turbidity of not more than about 150
Nephelometric Turbidity Units (NTU).
[0006] In another aspect, the invention relates to a liquid
concentrate or dry beverage composition that exhibits the above
characteristics upon dilution with the appropriate amount of
aqueous liquid (e.g. water) to provide a consumable beverage.
DETAILED DESCRIPTION OF THE INVENTION
A. Definitions
[0007] As used herein, the term "botanical flavor" or "botanical
extract" refers to flavors derived from parts of the plant other
than the fruit. As such, botanical flavors can include those
flavors derived from nuts, bark, roots and leaves. Also included
within this term are synthetically prepared flavors made to
simulate botanical flavors derived from natural sources. Examples
of botanical flavors include hibiscus, marigold, chrysanthemum and
the like. Botanical flavors can also be synthetically prepared.
[0008] As used herein, the term "caloric content" refers to the
total energy in kilocalories (kcal) per serving of consumable
beverage (250 mL) derived from the carbohydrate, protein, and lipid
components of the beverage. Caloric content is calculated using the
general factors of 4, 4, and 9 kcal per gram for the total level of
carbohydrate, protein, and lipid, respectively (United States Code
of Federal Regulations, Title 21, Section 101.9, Nutrition Labeling
of Food).
[0009] As used herein, the term "comprising" means various
components can be conjointly employed in the beverages of this
invention. Accordingly, the terms "consisting essentially of" and
"consisting of" are embodied in the term comprising.
[0010] As used herein, the terms "concentrated liquid composition"
and "concentrate" mean a liquid composition of the present
invention that is intended to be diluted with an aqueous liquid,
such as water, prior to consumption as a beverage. The skilled
artisan will recognize that the concentration of such compositions
will be dictated by the components contained therein and their
relative stability in an aqueous state. The concentrates of the
present invention are reconstituted with an aqueous liquid, such as
water, to provide a consumable beverage as described herein.
[0011] As used herein, the term "consumable beverage" and "final
beverage" are used interchangeably and refer to a beverage that is
prepared (e.g., diluted) in accordance with relevant package
labeling. Thus, as discussed below, a ready-to-drink beverage is
one that is sold such that it is consumed without additional
preparation by the consumer. In contrast, dry beverage compositions
and concentrates are intended to be diluted to provide a consumable
beverage.
[0012] As used herein, the term "dry beverage composition" means a
flowable particulate compositions that is substantially free of
moisture (e.g. a powder). Typically, such compositions will contain
not more than about 6% by weight total moisture. The dry beverage
compositions of the present invention are reconstituted with an
aqueous liquid, such as water, to provide a consumable beverage as
described herein.
[0013] As used herein, the term "juice" means whole, concentrated
or diluted juice from fruits and vegetables and other produce which
are squeezed or crushed to supply a beverage. Juice also refers to
citrus and non-citrus juices including vegetable juices.
[0014] As used herein the term "fruit flavors" refers to those
flavors derived from the edible reproductive part of the seed
plant, especially one having a sweet pulp associated with the seed,
for example, apples, oranges, lemon, limes, etc. Also included
within the term fruit flavor are synthetically prepared flavors
made to simulate fruit flavors derived from natural sources.
[0015] As used herein, the term "green tea catechins" refers to the
total content in parts per million (ppm) (or mg/L or .mu.g/mL) of
the following five catechins derived from green tea: epicatechin
(EC), epigallocatechin (EGC), epigallocatechin gallate (EGCG),
gallocatechin gallate (GCG), and epicatechin gallate (ECG).
[0016] As used herein, the term "nutritionally-supplemental amount"
is meant that the mineral (and any optional vitamin) sources used
in the practice of this invention provide a nourishing amount of
minerals and vitamins. This supplemental amount will provide from
about 5% to about 150% of the U.S. Reference Daily Intake (RDI).
The RDI for vitamins and minerals is as defined in the United
States of America (United States Code of Federal Regulations, Title
21, Section 101.9, Nutrition Labeling of Food).
[0017] As used herein, the term "polyvalent mineral cation" refers
to one or more minerals that typically exist in solution in the
form of positively charged cations with a net charge of +2 or
greater. Non-limiting examples of polyvalent mineral cations
include calcium (Ca.sup.2+), magnesium (Mg.sup.2+), manganese
(Mn.sup.2+), zinc (Zn.sup.2+), and iron (Fe.sup.2+, Fe.sup.3+).
[0018] As used herein, "ready-to-drink" (or "RTD") and
"ready-to-serve" are used interchangeably and refer to compositions
of the present invention that are at their recommended drink
strength and, therefore, are ready for consumption without the need
for reconstitution or dilution with aqueous liquids.
[0019] As used herein "single strength" refers to recommended drink
strength, i.e. the recommended concentration of the given beverage
composition.
[0020] As used herein the term "shelf stable" refers to packaged
beverages that do not require refrigeration while stored at ambient
temperatures for prolonged periods (e.g. more than 10 days).
[0021] As used herein, the term "solids" refers to the solid
materials extracted from the tea solutions which are soluble in
water. The solids include caffeine, flavanols, amino acids
(especially theanine), carbohydrates, edible acids, buffering
salts, proteins and related materials.
[0022] As used herein, the term "total insoluble calcium component"
refers to the aggregate of the moieties of a sample that bind to
calcium under the conditions described in the Analytical Methods
section below (Measurement of the Total Insoluble Calcium
Components) and thereby become insoluble in the sample.
[0023] As used herein, the term "vitamin C" refers to L-ascorbic
acid. The term "erythorbic acid" refers to its isomer,
D-isoascorbic acid.
[0024] As used herein, the term "water" includes any of tap,
filtered, purified, deionized, demineralized, distilled, spring,
mineral, artesian, softened, sparkling, or carbonated water.
[0025] All percentages are by weight unless otherwise
indicated.
B. Compositions
[0026] All concentration limits of components provided herein are
based on single strength beverages, unless otherwise stated.
[0027] As mentioned, the invention relates to RTD beverages, as
well as concentrated liquids and dry beverage compositions that
exhibit the above characteristics upon dilution with the
appropriate amount of aqueous liquid to provide a consumable
beverage. Thus, in the case of dry or concentrate compositions, it
will be recognized that the levels described presume that the dry
or concentrate composition is diluted to provide a consumable
beverage. That is, where catechin, polyvalent cation, turbidity,
etc. levels are stated with respect to a dry or concentrate
composition, those levels refer to the composition after it is
appropriately diluted to provide a consumable beverage.
[0028] The compositions of the present invention comprise a
significant level of green tea catechins, which are known to be
associated with various health benefits. Some of these health
benefits include cancer prevention, improved cardiovascular health,
and reduced blood pressure. The compositions of the present
invention comprise at least about 100 ppm of green tea catechins.
(Again, for compositions that are intended to be diluted prior to
consumption, the level of catechins stated herein assumes dilution
as appropriate for such consumable beverage.) In one aspect, the
beverage composition will comprise at least about 150 ppm green tea
catechins. In another aspect, the beverage composition will
comprise at least about 200 ppm green tea catechins. Preferably,
the beverage composition will comprise at least about 300 ppm green
tea catechins, and most preferably at least about 400 ppm green tea
catechins. Typically, the beverage composition will comprise from
about 100 to about 3,000 ppm green tea catechins.
[0029] The beverage compositions of the present invention have a
relatively high level of clarity (i.e. low turbidity). In this
regard, the compositions (in final, consumable form) will exhibit a
turbidity of not more than about 150 NTU. In another aspect, the
compositions will typically exhibit a turbidity of not more than
about 125 NTU, more typically not more than about 100 NTU.
Preferred beverage compositions of the present invention will
exhibit a turbidity of not more than about 50 NTU, even more
preferably not more than about 30 NTU. Typically, the beverage
compositions will exhibit a turbidity of from about 1 to about 150
NTU. Turbidity of the consumable beverages is measured with a
laboratory turbidimeter as described in the Analytical Methods
section.
[0030] The finished beverage compositions will comprise, on a 250
mL serving basis, at least about 10% of the RDI of one or more
polyvalent mineral cations. While the polyvalent mineral cation(s)
may be selected from a wide range of materials, the following
provides a non-exhaustive list of preferred cations. Preferred
polyvalent mineral cations may be selected from calcium, magnesium,
manganese, zinc, and/or iron (di- or trivalent), or mixtures
thereof. The RDI values for these minerals are as follows (United
States Code of Federal Regulations, Title 21, Section 101.9,
Nutrition Labeling of Food): calcium, 1000 mg; magnesium, 400 mg;
manganese, 2 mg; zinc, 15 mg; and iron, 18 mg. Suitable sources of
these minerals include, but are not limited to, the following
salts: citrate, sulfate, gluconate, lactate, bis-glycinate, amino
acid chelates, carbonate, oxide, hydroxide, chloride, phosphate,
pyrophosphate, acetate, fumarate, and malate. Preferred sources of
calcium are calcium citrate malate, calcium gluconate, calcium
lactate, and calcium lactate gluconate. Preferred sources of
magnesium are magnesium sulfate and magnesium gluconate. A
preferred source of zinc is zinc gluconate. A preferred source of
iron is the amino acid chelate iron bis-glycinate, available as
Ferrochel.RTM. from Albion Laboratories, Inc., Clearfield, Utah.
Another preferred source of iron is ferrous gluconate. Optionally,
other minerals can be added to the beverage compositions of the
present invention, including phosphorus, iodine, selenium, copper,
fluoride, chromium, molybdenum, sodium, potassium, and chloride. In
one aspect, the compositions will comprise, on a 250 mL serving
basis, at least about 15% of the RDI of one or more polyvalent
mineral cations. In yet another aspect, the compositions will
comprise, on a 250 mL serving basis, at least about 20% of the RDI
of one or more polyvalent mineral cations. Typically, the
compositions will comprise, on a 250 mL serving basis, from about
10% to about 150% of the RDI of one or more polyvalent mineral
cations. Of course, the dry and concentrate compositions of the
present invention will have mineral levels such that they provide
the above described ranges upon appropriate dilution to provide a
consumable beverage.
[0031] The compositions will preferably have, when in final form
for consumption, a pH of from about 2 to about 6.5. In one aspect,
the consumable beverage will have a pH of from about 2.5 to about
5, more preferably from about 3 to about 4.5. A pH within the most
preferred range of from about 3 to about 4.5 is particularly
desirable for minimizing dark color in a consumable beverage that
does not have added coloring agents. For example, applicants
surprisingly discovered that, even when iron is not part of the
formulation, green tea and mineral fortified water beverages are
characterized by significantly less brown color when the pH is
within the most preferred range. When iron is one of the fortifying
polyvalent mineral cations in the beverage formulation, low pH is
especially important for minimizing the interaction between the
iron cation and green tea polyphenol components, which yields
significant darkening of the beverage at higher pH.
[0032] The compositions of the present invention will preferably
exhibit low brown color, which is important to the ultimate
consumer. Brown color is characterized by measuring absorbance of
the consumable beverage at 430 nm as described in the Analytical
Methods section. (Again, it will be recognized that the absorbance
at 430 nm is measured using the consumable beverage. Thus, for
compositions that are intended to be diluted prior to consumption,
the absorbance characteristics stated herein assume dilution as
appropriate for such consumable beverage.) Absorbance at 430 nm
reflects the degree of brownish color in the beverage that can be
caused by the presence of theaflavins, thearubigins, proteins,
chlorophylls, and their degradation products. In one aspect, the
beverage compositions will preferably have an absorbance at 430 nm
of not more than about 0.15. In another aspect, the beverage
compositions will have an absorbance at 430 nm of not more than
about 0.12. In yet another aspect, the beverage compositions will
have an absorbance at 430 nm of not more than about 0.10.
Preferably, the beverage compositions will have an absorbance at
430 nm of not more than about 0.08, most preferably not more than
about 0.05. Typically, the beverage compositions will have an
absorbance at 430 nm of from about 0.01 to about 0.15.
[0033] It will be recognized that in addition to preferably being
low in brown color, by virtue of low absorbance at 430 nm, the
beverages of the present invention will also preferably be low in
color in general. As absorbance at 430 nm of the finished beverage
decreases, appearance of the beverage becomes more similar to water
and eventually the appearance becomes almost indistinguishable from
water. This is particularly true when the beverage is packaged in a
green colored glass or plastic bottle, as is often the case for
premium bottled waters (e.g. Perrier.RTM.).
[0034] Applicants have discovered that undesired solubility issues
associated with inclusion of calcium (often a preferred nutrient in
fortified beverages) in the present beverage compositions can be
addressed by limiting the level of total insoluble calcium
components, including oxalic acid, prior to calcium addition. As
such, compositions of the present invention that include calcium
will preferably contain not more than about 35 ppm oxalic acid or
salts thereof. More typically, the compositions will contain not
more than about 20 ppm, still more typically not more than about 7
ppm, oxalic acid or salts thereof. In addition, when calcium is
present in the beverage composition, the composition will
preferably contain not more than about 1000 ppm of total insoluble
calcium components including oxalic acid. More typically, the
compositions will contain not more than about 450 ppm, still more
typically not more than about 250 ppm, total insoluble calcium
components including oxalic acid. A preferred process for removing
total insoluble calcium components, including oxalic acid, to avoid
solubility issues is described below.
[0035] In a preferred process, tea extract is treated with a
soluble calcium source to remove insoluble calcium components
without affecting the level of catechins. The treatment is
typically carried out at ambient or higher temperatures, preferably
at temperatures greater than about 130.degree. F. (54.degree. C.).
More typically, the reaction temperature is greater than about
145.degree. F. (63.degree. C.), still more typically the reaction
temperature is greater than about 160.degree. F. (71.degree. C.).
The reaction time is typically about 2 hours or less. More
typically the reaction time is about 45 minutes or less; still more
typically the reaction time is about 15 minutes or less. The
preferred calcium salts to promote precipitation of the calcium
insoluble components are calcium sulfate, calcium chloride, calcium
acetate and calcium gluconate. Other sources of soluble calcium can
also be used. The preferred pH during the treatment is less than or
equal to about 7. The concentration of soluble calcium added to the
tea extract to promote precipitation of the calcium insoluble
components may vary from about 400 mg to about 10,000 mg per 100 gm
of tea extract on a dry weight basis. For conventional green tea
extracts, e.g. green tea powdered extract #285060 commercially
available from Plantextrakt, Inc. (Parsippany, N.J.), the amount of
calcium required tends to be toward the upper limit of this range
of addition. For nano-filtered tea extract, e.g. Green Power
SynerTea.TM. brand of green tea extract (commercially available
from Amax NutraSource, Inc., Eugene, Oreg.), the amount of calcium
required tends to be toward the lower limit of this range of
addition. This is because the nanofiltration process used during
manufacture of the SynerTea.TM. brand of green tea extract removes
a portion of the higher molecular weight calcium insoluble
components, such as pectin. After treatment to precipitate the
calcium insoluble components, the tea extract is filtered to remove
the insoluble/suspended material. The preferred level of insoluble
calcium components in the treated green tea extract, on a dry
weight basis, is not more than about 1% w/w. More typically, the
level of insoluble calcium components is not more than about 0.6%
w/w; still more typically the level is not more than about 0.1%
w/w.
[0036] In a related aspect, applicants have surprisingly discovered
that the solubility issues associated with calcium addition are not
encountered with other polyvalent mineral cations. As such, it
surprisingly does not appear that additional processing of the
green tea (i.e., to reduce oxalic acid/pectin levels) is necessary
when soluble polyvalent mineral cations other than calcium are
included in the present compositions.
[0037] The beverage compositions of the present invention will
preferably have a relatively low caloric content. In one preferred
aspect of the invention, the compositions will have a caloric
content, on a 250 mL serving basis, of not more than about 60
kilocalories (kcal). In another aspect, the compositions will
typically have a caloric content, on a 250 mL serving basis, of not
more than about 30 kcal, preferably not more than about 15 kcal. In
a similar regard, the beverage compositions will preferably have a
relatively low carbohydrate level. As such, in one preferred
aspect, the compositions will have a carbohydrate level, on a 250
mL serving basis, of not more than about 15 g, preferably not more
than about 8 g, still more preferably not more than about 4 g.
[0038] The beverage compositions of the present invention, when in
the form of a liquid concentrate or a RTD beverage, comprise water.
Ready-to-drink beverages typically contain from about 80% to about
99.8% water. Preferably the water is soft, demineralized, or
deionized. Concentrates of the present invention typically contain
from about 20% to about 79%, more typically from about 30% to about
70% water. If desired, the water used in the beverage formulation
may be carbonated; e.g. sparkling or carbonated water. More
typically, a carbonated beverage is produced by solubilizing carbon
dioxide gas into the final blended beverage. Usually a beverage
will be considered carbonated if it comprises more than 30%,
preferably more than 100%, by volume of solubilized carbon dioxide.
Carbonated beverages typically comprise from 100% to 450%,
preferably from 200% to 350%, carbon dioxide by volume of the
beverage.
[0039] The beverage compositions of the present invention comprise
green tea extract. The extract can be obtained from either a single
tea plant or a mixture of plants and it can be in the form of a
liquid extract or a dry powdered extract. It is preferred that the
green tea extract be light in color and enriched in unoxidized
flavanols, i.e., catechin monomers. Preferably, the green tea
extract comprises at least about 10% green tea catechins on a dry
solids basis, more preferably at least about 20% catechins.
Non-limiting examples of suitable green tea extracts include Green
Power SynerTea.TM. brand of green tea extract (commercially
available from Amax NutraSource, Inc., Eugene, Oreg.), green tea
powdered extract #285060 commercially available from Plantextrakt,
Inc. (Parsippany, N.J.), and green tea extracts produced by the
processes described in U.S. Pat. No. 5,879,733 issued to Ekanayake,
et al. (1999) and U.S. Pat. No. 5,427,806 issued to Ekanayake, et
al. (1995). Preferred green tea extracts to use when calcium is not
included in the beverage formulation are the Green Power
SynerTea.TM. brand of green tea extract and/or the extract prepared
according to the process described in U.S. Pat. No. 5,879,733. A
preferred green tea extract when calcium is included in the
beverage compositions of the present invention is the extract
prepared according to the process described above, in which the
extract has been treated to remove insoluble calcium components,
such as oxalic acid and pectin. The level of green tea extract in
the beverage compositions of the present invention may vary, as
long as the beverage comprises at least about 100 ppm of green tea
catechins. Typically, the consumable beverages of the present
invention will comprise from about 0.03% to about 1% green tea
extract solids, more typically from about 0.08% to about 0.5%.
[0040] In one aspect of the present invention, the beverage
composition preferably comprises food-grade acids to reduce the pH
of the beverage. The inventors surprisingly discovered that
addition of acid to reduce the pH of the consumable beverage
results in a lower absorbance at 430 nm, i.e. the beverage is less
brown in color. Non-limiting examples of food-grade acids that can
be used to reduce the pH of the beverage include citric, malic,
phosphoric, tartaric, ascorbic, and erythorbic acids. Another
benefit associated with the addition of food-grade acids to the
present beverage composition is improved color stability of the
beverage during storage. It is known that the brown color of tea
beverages results from oxidation of the catechin monomers to yield
high-molecular weight polymers (i.e., theaflavins and
thearubigins). Oxidation of the catechins can be controlled and,
hence, browning of the green tea beverage delayed or prevented by
the addition of acids such as citric, ascorbic, and erythorbic
acids. While not wishing to be bound by theory, it is believed that
citric acid helps prevent oxidation of the green tea catechins by
lowering the beverage pH and by complexing metal ions such as iron
and copper, which are known to be oxidation catalysts. It is
believed that ascorbic and erythorbic acids help prevent oxidation
of the catechins because they are effective reducing agents. The
preferred food-grade acids for use in the beverage compositions of
the present invention are citric, malic, ascorbic, and/or
erythorbic acids.
[0041] Other optional ingredients in the beverage compositions of
the present invention include carbohydrate sweeteners, zero or low
calorie high-intensity or artificial sweeteners, soluble fibers and
polysaccharides, proteins and/or peptides, amino acids,
emulsifiers, vitamins, salts, natural and/or artificial flavoring
agents, flavor enhancers, caffeine, preservatives, and natural
and/or artificial coloring agents or other ingredients.
[0042] The beverage compositions of the present invention can
optionally contain a natural and/or artificial flavoring agent. The
particular amount of flavoring agent effective for imparting flavor
characteristics to the beverage depends upon the flavor(s)
selected, the flavor impression desired and the form of the flavor.
The flavoring agent can comprise a fruit juice or vegetable juice,
a fruit or vegetable flavor or mixtures thereof. The juice can be
provided as juice made from, for example, apple, cranberry, pear,
peach, plum, apricot, nectarine, grape, cherry, currant, raspberry,
gooseberry, blackberry, blueberry, strawberry, lemon, lime,
mandarin, orange, grapefruit, potato, tomato, lettuce, celery,
spinach, cabbage, watercress, dandelion, rhubarb, carrot, beet,
cucumber, pineapple, coconut, pomegranate, kiwi, mango, papaya,
banana, watermelon, tangerine and cantaloupe. Preferred juices are
apple, pear, lemon, lime, mandarin, grapefruit, cranberry, orange,
strawberry, tangerine, grape, kiwi, pineapple, passion fruit,
mango, guava, raspberry and cherry. Citrus juices, such as
grapefruit, orange, lemon, lime, mandarin and juices of mango,
passion fruit and guava, or mixtures thereof, are most
preferred.
[0043] The fruit or vegetable juice(s) are present in an amount of
from 0% to about 95%, preferably from 0% to about 35%, and more
preferably from 0% to about 10% of the beverage. This concentration
is based on the single strength of the beverage.
[0044] The flavoring agent according to the present invention can
also comprise flavors selected from fruit flavors, botanical
flavors, vegetable flavors and mixtures thereof. Particularly
preferred fruit flavors are the citrus flavors including orange
flavors, lemon flavors, lime flavors and grapefruit flavors.
Besides citrus flavors, a variety of other fruit flavors can be
used such as apple flavors, grape flavors, cherry flavors,
pineapple flavors and the like. These fruit flavors can be derived
from natural sources such as fruit juices and flavor oils, or else
be synthetically prepared. Particularly preferred botanical flavors
are hibiscus, marigold and chrysanthemum.
[0045] The flavor agent can also comprise a blend of various
flavors, e.g., lemon and lime flavors, citrus flavors and selected
spices (the typical cola soft drink flavor) etc. If desired the
flavor can be formed into emulsion droplets and then dispersed in
the beverage drink. Because these droplets usually have a specific
gravity less than that of water and would therefore form a separate
phase, weighting agents (which can also act as clouding agents) can
be used to keep the emulsion droplets dispersed in the beverage.
Examples of such weighting agents are sucrose acetate isobutyrate,
brominated vegetable oils (BVO) and resin esters, in particular the
ester gums. See L. F. Green, Developments in Soft Drinks
Technology, Vol. 1 (Applied Science Publishers Ltd. 1978) pp. 87-93
for a further description of the use of weighting and clouding
agents in liquid beverages.
[0046] Flavoring agents which are not substantially juice, comprise
no more than about 3% of the beverage, preferably such flavor
component comprises at least 0.001% by weight of the beverage and
typically from about 0.01% to about 3% by weight of the
beverage.
[0047] The beverage compositions of the present invention can
optionally contain preservatives such as benzoic acid, sorbic acid,
and salts thereof; salts such as sodium chloride, potassium
chloride, sodium phosphate, potassium phosphate, sodium citrate,
and potassium citrate; polysaccharides and/or soluble fibers such
as guar gum, xanthan gum, alginates, starches, pectin,
maltodextrins, gum arabic, arabinogalactan, inulin,
fructooligosaccharide, and polydextrose; proteins such as milk
proteins (caseins and/or whey proteins) and soy protein;
emulsifiers such as mono- and di-glycerides and lecithin; and
vitamins such as vitamins C, A, D, E, K, and the B-complex vitamins
B1 (thiamine), B2 (riboflavin), B3 (niacin), B6 (pyridoxine), B12
(cyanocobalamin), and folic acid.
[0048] The beverage compositions of the present invention are
produced by combining the appropriate ingredients using standard
beverage manufacturing and processing procedures. For example, see
The Chemistry and Technology of Soft Drinks and Fruit Juices (P. R.
Ashurt, Editor, CRC Press, 1998). In making a single strength
beverage, a liquid concentrate or syrup is usually formed first.
This liquid concentrate typically contains flavoring agents and/or
fruit juice concentrates, acids, salts, high-intensity sweeteners
if used, and suitable preservatives if needed. The liquid
concentrate usually contains from about 30% to about 70% by weight
water. The ingredients are added to the water and mixed in
conventional equipment. If desired, the green tea extract can also
be incorporated into the liquid concentrate or, alternatively, the
green tea extract may be added to the final blended beverage just
prior to packaging. After the concentrate is formed, additional
carbohydrate sweetener may be added and water is added to make a
finished consumable beverage ready for packaging. The product may
be cold-filled or hot packed into a suitable container.
C. Analytical Methods
1. Measurement of the Green Tea Catechin Level:
[0049] The total level of green tea catechins in consumable
beverages or aqueous tea extracts is measured using the following
method. [0050] a) Reference: [0051] A. Finger et al.,
"Chromatography of tea constituents", J. Chromatogr., (1992), 624:
293-315. [0052] b) Scope: [0053] This method is used to measure the
level of green tea catechins in consumable beverages. Five green
tea catechins (EC, EGC, EGCG, GCG, and ECG) are measured in the
beverage using linear response plots prepared with individual pure
standards. This method is also used to measure the level of green
tea catechins in aqueous tea extracts after dissolving or diluting
the tea extract in water to achieve approximately 0.15% tea solids.
[0054] c) Principle: [0055] The consumable beverage is usually
diluted 1:10 or 1:100 with diluent (see below) to obtain signals
lying within the range of the calibration curve. The diluted sample
is filtered through a 0.2 .mu.m filter to remove particulates. The
sample is then injected onto a C-18 reversed phase High Performance
Liquid Chromatography (HPLC) column. The catechins are eluted using
a gradient mobile phase composed of a 0.01 M phosphate buffer at pH
3.1 and acetonitrile. Detection is performed using a UV absorbance
detector set to 280 nm. [0056] d) Apparatus: [0057] Class A
volumetric flasks (1000 mL, 10 mL, 5 mL) [0058] Sartorius four
place balance [0059] Supelco vacuum filtration unit [0060] HP auto
sampler vials [0061] Whatman Anotop 25 (0.2 .mu.m) inorganic
membrane filter [0062] 5 mL disposable syringe
TABLE-US-00001 [0062] Instrument Set-up Agilent-1090 HPLC Agilent
1090 Diode Array Detector set to 280 nm Agilent Chemstation for LC,
Rev. A.04.02 YMC basic column 250 mm .times. 2 mm 5 .mu.m, serial
#: 112099G
[0063] e) Reagents: [0064] Acetonitrile (HPLC grade, J. T. BAKER,
cat# 9011-03, lot N42B26) [0065] Milli-Q water with resistance
greater than or equal to 18 M.OMEGA.-cm [0066] EDTA (Fisher
Scientific, cat#. S311, lot 860954) [0067] Phosphoric acid (J. T.
BAKER, cat# 0260-01, lot 25806) [0068] Potassium dihydrogen
phosphate (J. T. BAKER, cat# 4008-01, lot 30K0178)) [0069] Sodium
bisulfite (Sigma, cat#. S9000, lot 30K0178) [0070] Caffeine (CF,
Sigma, cat#. C0750, lot 127F-0395) [0071] Epigallocatechin (EGC,
Sigma, cat#. E3768, lot 61K1428) [0072] Epicatechin (EC, Sigma,
cat#. E1753) [0073] Epigallocatechingallate (EGCG, Sigma, cat#.
E4143, lot 61K1773) [0074] Epicatechingallate (ECG, Sigma, cat#.
E3893, lot 31K1236) [0075] Gallocatechin gallate (GCG, Sigma, cat#.
G6782, lot 110K1413) [0076] f) Solutions: [0077] 0.01 M (1.36 g/L)
potassium dihydrogen phosphate buffer: [0078] Weigh 1.36 g
potassium dihydrogen phosphate into a 1 liter volumetric flask. Add
approximately 600 mL HPLC grade water and stir until solid is
dissolved. Titrate with phosphoric acid to a pH of 3.1. Bring to
volume with HPLC grade water. Degas using vacuum filtration system.
[0079] Diluent: [0080] Use to dilute the sample and ensure
stability of the catechins under ambient conditions. Add 0.24 g
EDTA and 1.24 g sodium bisulfite (NaHSO.sub.3) to 910 mL of 0.01M
potassium dihydrogen phosphate buffer. Add 90 mL of acetonitrile.
[0081] Preparation of Beverage Sample: [0082] Typically, pipet 0.5
mL of a finished beverage into a 5 mL volumetric flask (1:10
dilution) or 0.1 mL of a finished beverage into a 10 mL volumetric
flask (1:100 dilution) and bring to volume with diluent. Filter the
resulting solution through a 0.2 .mu.m Whatman filter. Transfer the
filtered sample to the auto sampler vial. [0083] Preparation of
Standard Solutions: [0084] Each pure standard (caffeine and the
five catechins) is accurately weighed and placed into a 5 mL or 10
mL volumetric flask as shown below. Add diluent to dissolve the
standard and fill the flask to volume. These are standard stock
solutions (.about.1000 ppm). Standard working solutions are then
prepared by diluting the standard stock solutions with diluent. The
actual weights and concentrations of the standard stock solutions
and working solutions are shown in the following Table.
TABLE-US-00002 [0084] EGC CF EC EGCG GCG ECG Volume (mL) 5 10 10 5
5 5 Actual 0.0043 0.0105 0.0940 0.0049 0.0045 0.0044 weights (g)
Stock 860 1050 940 980 900 880 Solution (.mu.g/mL) Working 172 420
188 196 180 176 Solution (.mu.g/mL)
[0085] Using the standard working solutions, response factor
mixtures are prepared as shown below:
TABLE-US-00003 [0085] .mu.L of Standard Working Solution Mixture
Caf- .mu.L Total # EGC feine EC EGCG ECG GCG Diluent .mu.L 6 600
400 250 100 250 250 3150 5000 7 500 500 20 300 150 20 3510 5000 8
400 25 100 1200 200 100 2975 5000 9 150 300 200 900 20 200 3230
5000 10 50 100 300 650 300 300 3150 5000
[0086] The actual concentrations of each standard (caffeine and the
5 catechins) in the response factor mixtures are as follows:
TABLE-US-00004 [0086] Concentration of Standards (.mu.g/mL) Mixture
# EGC Caffeine EC EGCG ECG GCG 6 20.64 33.6 9.4 3.92 8.8 9.0 7 17.2
42 0.75 11.76 5.28 0.72 8 13.76 2.1 3.76 47.04 7.04 3.6 9 5.16 25.2
7.52 35.28 0.704 7.2 10 1.72 8.4 11.28 31.36 10.56 10.8
[0087] g) Chromatography Conditions: [0088] Sample size--25 .mu.L
[0089] Detector--280 nm AUFS 0.100 [0090] Mobile Phase: [0091]
A=water [0092] B=0.01M potassium dihydrogen phosphate buffer, pH
3.1 [0093] C=Acetonitrile [0094] Gradient:
TABLE-US-00005 [0094] 0 min. 1% A + 90% B + 9% C 15 min. 2% A + 80%
B + 18% C 18 min. 3% A + 70% B + 27% B 30 min. 1% A + 90% B + 9% C
45 min. stop
[0095] Flow rate: 0.4 mL/min [0096] h) Calculation of Catechin
Level in the Consumable Beverage: [0097] Peak areas corresponding
to each catechin standard on the HPLC chromatogram of the response
factor mixtures are used to prepare a linear response plot for each
catechin. The correlation coefficients (r-square) for each response
plot are typically equal to or greater than 0.99. The beverage
sample chromatogram is analyzed for the peak area of each catechin.
The level of catechins in the beverage sample is determined from
the linear response plots. The level of catechins in the consumable
beverage is then calculated by multiplying by the dilution factor
used (10.times. or 100.times.). The total level of green tea
catechins in ppm (.mu.g/mL or mg/L) in the finished beverage is
calculated by adding the levels of the five individual catechins
measured (EGC+EC+EGCG+ECG+GCG).
2. Measurement of the Turbidity of Consumable Beverages:
[0097] [0098] A Hach Model 2100AN Turbidimeter (Hach Company,
Loveland, Colo.) is used to measure the turbidity of consumable
beverages. This instrument measures the turbidity of liquids in
Nephelometric Turbidity Units (NTU). The turbidimeter is first
calibrated with a set of Gelex.RTM. Secondary Turbidity Standards.
Measurements are made using the following instrument parameters:
ratio on; signal averaging on; automatic range selection; US EPA
filter installed. The beverage is equilibrated to room temperature
and then poured into a turbidimeter sample cell (sample cell outer
diameter=25 mm). The sample cell is inserted into the instrument
and the turbidity reading (NTU) is recorded after waiting 30-60
seconds for the reading to stabilize. The measured NTU value is
indicative of the level of turbidity of the consumable beverage.
Higher NTU values indicate greater turbidity.
3. Measurement of Absorbance at 430 nm of Consumable Beverages:
[0098] [0099] A UV-Visible spectrophotometer (Unicam UV1 UV-Visible
Spectrometer; Unicam Limited, Cambridge, United Kingdom) is used to
measure absorbance at 430 nm of consumable beverages. The beverage
is equilibrated to room temperature and then poured into a sample
cuvette (1 cm path length), which is placed in the sample holder of
the spectrophotometer. A blank cuvette filled with deionized water
is placed in the blank holder of the spectrophotometer. Absorbance
of the beverage sample at a wavelength of 430 nm is measured and
recorded (A). The cuvette in the sample holder is then replaced
with another blank cuvette filled with deionized water and
absorbance of the blank measured at 430 nm and recorded (B). The
absorbance of the beverage sample is then adjusted by subtracting
the measured absorbance of the deionized water blank:
[0099] Absorbance at 430 nm=(A)-(B) [0100] This procedure corrects
for any measured absorbance contributed from the water. In theory,
absorbance of the deionized water blank (B) will approach zero. The
absorbance at 430 nm is indicative of the level of brown color in
the beverage.
4. Measurement of pH:
[0100] [0101] The pH of consumable beverages and aqueous tea
extracts is measured with a Corning Model 440 pH Meter. Prior to
making pH measurements, the meter is calibrated using pH 4.00 and
7.00 standard buffer solutions (VWR Scientific, West Chester,
Pa.).
5. Measurement of the Level of Polyvalent Mineral Cations in
Consumable Beverages:
[0101] [0102] Levels of the minerals calcium, magnesium, manganese,
zinc, and iron in consumable beverages are measured by Inductively
Coupled Plasma Emission Spectrometry according to the methods
described in the following references: [0103] a) "Inductively
Coupled Plasma-Atomic Emission Spectrometry Analysis of Biological
Materials and Soils for Major, Trace, and Ultra-Trace Elements",
Applied Spectroscopy, volume 32, pg. 1-29, 1978. [0104] b) AOAC
Official Method 985.01, "Metals and Other Elements in Plants and
Pet Foods", (3.2.06, Chp. 3, pg. 4). [0105] c) AOAC Official Method
984.27, "Calcium, Copper, Iron, Magnesium, Manganese, Phosphorus,
Potassium, Sodium, and Zinc in Infant Formula", (50.1.15, Chp. 50,
pg. 15-16). [0106] All AOAC (Association of Official Analytical
Chemists) published methods can be found in the following
reference: [0107] AOAC International, Official Methods of Analysis,
P. Cunniff (ed.), 16.sup.th edition, 5.sup.th Revision, 1999,
Gaithersburg, Md. [0108] The level of each mineral is expressed as
mg per 250 mL of beverage. The % RDI of each mineral is calculated
by dividing the mineral level by the respective RDI value:
[0108] % RDI=[(mg/250 mL beverage)/(RDI)].times.100 [0109] The RDI
values for the minerals are as follows (United States Code of
Federal Regulations, Title 21, Section 101.9, Nutrition Labeling of
Food): calcium=1,000 mg; magnesium=400 mg; manganese=2 mg; zinc=15
mg; iron=18 mg.
6. Measurement of the Caloric Content and Carbohydrate Content of
Consumable Beverages:
[0109] [0110] Caloric content in kilocalories (kcal) per 250 mL of
beverage is determined from the carbohydrate, protein, and lipid
contents of the beverage. Caloric content is calculated using the
general factors of 4, 4, and 9 kcal/g for the content of
carbohydrate, protein, and lipid, respectively, per 250 mL serving
of beverage (United States Code of Federal Regulations, Title 21,
Section 101.9, Nutrition Labeling of Food):
[0110] Caloric Content(kcal/250 mL beverage)=[(g carbohydrate/250
mL).times.4]
+[(g protein/250 mL).times.4]+[(g lipid/250 mL).times.9] [0111]
Protein content (g/250 mL beverage) is measured according to the
following method (a conversion factor of 6.25 is used to convert %
nitrogen to % protein): [0112] AOAC Official Method 968.06,
"Protein (Crude) in Animal Feed" (modified), Official Methods of
Analysis, Patricia Cunniff (Ed.), 16.sup.th edition, Vol. 1, AOAC
International, Gaithersburg, Md. (1995). [0113] Lipid content
(g/250 mL beverage) is measured by acid hydrolysis according to the
following method: [0114] AOAC Official Method 954.02, Official
Methods of Analysis, 17.sup.th edition, Vol. 1, AOAC International,
Gaithersburg, Md. (2000). [0115] Ash content (g/250 mL beverage) is
measured according to the following method: [0116] AOAC Official
Method 923.03, "Ash of Flour" (modified), Official Methods of
Analysis, Patricia Cunniff (Ed.), 16.sup.th edition, Vol. 2, AOAC
International, Gaithersburg, Md. (1995). [0117] Moisture content
(g/250 mL beverage) is measured according to the following method:
[0118] AOAC Official Method 934.06, "Moisture in Dried Fruits"
(modified), Official Methods of Analysis, Patricia Cunniff (Ed.),
16.sup.th edition, Vol. 2, AOAC International, Gaithersburg, Md.
(1995). [0119] Carbohydrate content is calculated by difference
using the following equation:
[0119] Carbohydrate Content(g/250 mL beverage)=100-(Protein
Content)-(Lipid Content)-
(Ash Content)-(Moisture Content)
7. Measurement of the Moisture Content of Dry Beverage
Compositions:
[0120] Moisture content of dry beverage compositions is measured
according to the following method: AOAC Official Method 979.12,
"Moisture (Loss on Drying) in Roasted Coffee", Official Methods of
Analysis, Patricia Cunniff (Ed.), 16.sup.th edition, 5.sup.th
revision, AOAC International, Gaithersburg, Md. (1999).
8. Measurement of the Oxalic Acid Level:
[0120] [0121] This method is used to measure the level of oxalic
acid in consumable beverages and aqueous tea extracts. [0122] a)
Reference: [0123] Official Methods of Analysis of AOAC
INTERNATIONAL (2000) 17.sup.th Ed. AOAC INTERNATIONAL,
Gaithersburg, Md., USA, Official Method 986.13. (modified) [0124]
b) Scope: [0125] This method is used to measure the level of oxalic
acid, fumaric acid, tartaric acid, citric acid, malic acid, lactic
acid, succinic acid, and acetic acid in food products. [0126] c)
Principle: [0127] The sample is filtered to remove interferences.
Organic acids are then separated using HPLC utilizing UV detection
at 214 nm. [0128] d) Apparatus: [0129] Class A volumetric flasks
(1000 mL, 10 mL, 5 mL) [0130] Sartorius four place balance [0131]
Liquid Chromatograph--System equipped with Model 7725i inhector,
Model 2487 variable wavelength detector operable at 214 nm, 0.1
AUFS (Waters Associates, Inc.) and computing integrator
(Hewlett-Packard Integrator 3390 [replaced by No. 3396B], or
equivalent). [0132] Analytcal Columns--(1) Supelcosil LC-18, or
equivalent, 5 .mu.m particle size, 25 cm.times.4.6 mm, in tandem
with and followed by (2) Radial-Pak C18 cartridge (Water Associate,
Inc.), 5 .mu.m particle size, 10 cm long, used with Radial
Compression Module. Radial-Pak C18 cartridge can be substituted by
any standard 25 or 30 cm stainless steel reverse phase C18 column
with 10 .mu.m particle size. Connect Bio-Rad reverse phase
micro-guard column (ODS-10) ahead of column 1. Mobile phase:
phosphate buffer at 0.8 mL/min; sensitivity 0.1 AUFS. [0133] e)
Disposable cartridges:--Sep-Pak C18 (Water Associates, Inc.) [0134]
0.45 .mu.m inorganic membrane filter [0135] f) Reagents: [0136]
Potassium phosphate monobasic (KH.sub.2PO.sub.4) [0137] 85%
Phosphoric acid [0138] Methanol [0139] CH.sub.3CN [0140] Malic acid
Standard ACS grade [0141] Citric acid Standard ACS grade [0142]
Oxalic acid Standard ACS grade [0143] Quinic acid Standard ACS
grade [0144] g) LC mobile phase: [0145] 0.2 M Phosphate buffer, pH
2.4:-- [0146] Weigh 27.2 g potassium dihydrogen phosphate in
beaker. Add water to 950 mL. Using pH meter and 85% phosphoric
acid, adjust to pH 2.4. Pour into 1 L graduate and adjust to volume
with water; filter. [0147] Preparation of Test Samples and
Standards [0148] (a) Working standard solutions.--Weigh 0.200 g
each of ACS grade quinic, malic, citric, and oxalic acids to the
nearest 0.1 mg. Dissolve in water, make up the volume to 100 mL in
a volumetric flask with water and filter. [0149] (b) Test sample
solutions.--Cartridge is conditioned by eluting 10 mL
CH.sub.3CN--H.sub.2O (50+50) through 10 mL Luer-Lok syringe. The
syringe is removed and 10 mL air is passed through the cartridge.
Ten mL of sample is eluted through the conditioned cartridge. First
4-5 mL is discarded and the next 4-5 mL is collected and filtered
for LC analysis. [0150] Determination: [0151] The system is
conditioned with 100% methanol (or methanol-H.sub.2O[70+30])
followed by water and then phosphate buffer. The order is reversed
at end of working day; never letting methyl alcohol to come in
contact with phosphate buffer. Operating conditions:--flow rate
0.80 mL/min; 214 nm detector; temperature ambient; sensitivity 0.1
AUFS. Column system is satisfactory when baseline separation is
achieved between sugar front peak and quinic acid in aqueous green
tea extract. 5-20 .mu.L standard solution is injected after each 2
test sample injections to check linearity. 5 .mu.L test sample
solution is injected. An average of 2 injections are recorded for
standard and test sample responses. [0152] h) Calculations of
Oxalic acid
[0152] % Oxalic acid=(PA/PA').times.(V'/V).times.C where PA and
PA'=peak area of test sample and standard, respectively; V and
V'=volume of test sample and standard, respectively; and
C=concentration of standard, %.
9. Measurement of the Total Insoluble Calcium Components:
[0153] This method is used to measure the level of total insoluble
calcium components in consumable beverages or aqueous tea extracts.
Weigh 1000 g of the consumable beverage or 100 g of a 5% w/w
aqueous solution of green tea extract in a 2000 mL beaker. Add 20
mL of a 10% calcium chloride solution. Allow to stand for 1 hour
and then heat to 80.degree. C. and hold for 30 minutes. Filter
through a tared filter paper. Wash the gelatinous precipitate with
boiling water. Then dry and weigh the precipitate as total
insoluble calcium components.
D. EXAMPLES
Example 1
[0154] A green tea fortified water beverage of the present
invention is prepared according to the following formulation
TABLE-US-00006 Ingredient Wt. % g/L Deionized Water 96.582 989.1
Magnesium Sulfate, anhydrous (Tangram Co.; 0.086 0.88 Holtsville,
NY) .sup.1 Vitamin Premix (Roche Vitamins, Inc.; 0.029 0.30
Parsippany, New Jersey) .sup.2 Sucrose, granulated (The Amalgamated
Sugar 2.682 27.47 Co.; Ogden, Utah) Acesulfame Potassium
(Nutrinova, Inc.; 0.013 0.13 Somerset, New Jersey) Sodium Citrate,
dihydrate (A. E. Staley; 0.155 1.59 Decatur, Illinois)
Mono-potassium Phosphate (Astaris LLC; 0.086 0.88 Carteret, New
Jersey) Green Tea Extract Powder (SynerTea .TM.; 0.147 1.50 Amax
NutraSource, Inc.; Eugene, Oregon) Citric Acid, anhydrous (A. E.
Staley; 0.220 2.25 Decatur, Illinois) TOTAL = 100.0 1,024.1 .sup.1
Magnesium sulfate is 20.2% Mg .sup.2 The vitamin premix provides
the following nutrients per 250 mL serving of beverage: Vitamin C
22.2 mg Niacin 2.6 mg Vitamin B6 0.26 mg Vitamin B12 0.79 .mu.g
Vitamin E 3.96 International Units Zinc 1.74 mg
[0155] The source of zinc in the vitamin premix is zinc gluconate
(13.4% Zn).
[0156] The dry ingredients are weighed out and added to the
deionized water with agitation. Mixing is continued until all the
ingredients are in solution. The final beverage is clear with
minimal brown color and no turbidity. The beverage has the
following attributes:
TABLE-US-00007 Green Tea Catechin Level (ppm = mg/L) 400 ppm
Turbidity 22.3 NTU Absorbance at 430 nm (average of 2 0.043
measurements) pH 3.61 Mineral Levels (per 250 mL beverage):
Magnesium 44 mg = 11.0% RDI Zinc 1.7 mg = 11.3% RDI Carbohydrate
Content (per 250 mL beverage) 7 g Calorie Content (per 250 mL
beverage) 28 kcal
[0157] The beverage is packaged in green colored plastic bottles.
The in-package appearance is virtually identical to pure water.
Example 2
[0158] Two water beverage formulations fortified with green tea
extract are prepared according to the following formulations:
TABLE-US-00008 Formula A Grams/ Ingredient Wt. % Liter Deionized
Water 97.113 994.53 Magnesium Sulfate, anhydrous (Tangram Co.;
0.086 0.88 Holtsville, NY) .sup.1 Zinc Gluconate (Glucona America,
Inc.; 0.009 0.09 Janesville, Wisconsin) .sup.2 Sucrose, granulated
(The Amalgamated Sugar 2.682 27.47 Co.; Ogden, Utah) Acesulfame
Potassium (Nutrinova, Inc.; 0.013 0.13 Somerset, New Jersey) Green
Tea Extract Powder (Product #285060; 0.098 1.00 Plantextrakt, Inc.,
Parsippany, New Jersey) TOTAL = 100.0 1,024.1
TABLE-US-00009 Formula B Grams/ Ingredient Wt. % Liter Deionized
Water 96.652 989.81 Magnesium Sulfate, anhydrous (Tangram Co.;
0.086 0.88 Holtsville, NY) .sup.1 Zinc Gluconate (Glucona America,
Inc.; 0.009 0.09 Janesville, Wisconsin) .sup.2 Sucrose, granulated
(The Amalgamated Sugar 2.682 27.47 Co.; Ogden, Utah) Acesulfame
Potassium (Nutrinova, Inc.; 0.013 0.13 Somerset, New Jersey) Sodium
Citrate, dihydrate (A. E. Staley; 0.155 1.59 Decatur, Illinois)
Mono-potassium Phosphate (Astaris LLC; 0.086 0.88 Carteret, New
Jersey) Green Tea Extract Powder (Product #285060; 0.098 1.00
Plantextrakt, Inc., Parsippany, New Jersey) Citric Acid, anhydrous
(A. E. Staley; 0.220 2.25 Decatur, Illinois) TOTAL = 100.0 1,024.1
.sup.1 Magnesium sulfate is 20.2% Mg .sup.2 Zinc gluconate is 13.4%
Zn
[0159] Each beverage is prepared by weighing out the appropriate
amount of dry ingredients and adding the dry ingredients to the
deionized water with agitation. Mixing is continued until all the
ingredients are in solution. The final beverages have the following
attributes:
TABLE-US-00010 Formula A Formula B Green Tea 150 ppm 150 ppm
Catechin Level (ppm = mg/L) Turbidity 15.3 NTU 4.1 NTU Absorbance
at 430 0.302 0.129 nm (average of 2 measurements) pH 5.22 3.60
Mineral Levels (per 250 mL): Magnesium 44 mg = 11.0% RDI 44 mg =
11.0% RDI Zinc 3.0 mg = 20% RDI 3.0 mg = 20% RDI
[0160] Formula B has a lower pH and yields a final beverage with a
significantly lower absorbance at 430 nm and less visually apparent
brown color, relative to formula A.
Example 3
[0161] A fortified sports drink of the present invention is
prepared according to the following formulation.
TABLE-US-00011 Grams/ Ingredient Wt. % Liter Deionized Water 93.279
955.27 Magnesium Sulfate, anhydrous (Tangram Co.; 0.154 1.58
Holtsville, NY) .sup.1 Zinc Gluconate (Glucona America, Inc.; 0.009
0.09 Janesville, Wisconsin) .sup.2 Ferrous bis-glycinate (Ferrochel
.RTM., Albion 0.004 0.04 Laboratories, Inc., Clearfield, Utah)
.sup.3 Maltodextrin, 15 DE (Maltrin M150, Grain 3.095 31.70
Processing Corp., Muscatine, Iowa) Sucrose, granulated (The
Amalgamated Sugar 2.682 27.47 Co.; Ogden, Utah) Acesulfame
Potassium (Nutrinova, Inc.; 0.013 0.13 Somerset, New Jersey) Sodium
Citrate, dihydrate (A. E. Staley; 0.155 1.59 Decatur, Illinois)
Sodium Chloride (IMC Salt, Inc.; Overland 0.033 0.34 Park, Kansas)
Mono-potassium Phosphate (Astaris LLC; 0.086 0.88 Carteret, New
Jersey) Green Tea Extract Powder (SynerTea .TM.; 0.110 1.13 Amax
NutraSource, Inc.; Eugene, Oregon) Citric Acid, anhydrous (A. E.
Staley; 0.244 2.50 Decatur, Illinois) FD&C Red No. 40 powder
(B. F. Goodrich, 0.005 0.05 Cleveland, Ohio) Natural Flavor (Mane,
Inc., Milford, Ohio) 0.130 1.33 TOTAL = 100.0 1,024.1 .sup.1
Magnesium sulfate is 20.2% Mg .sup.2 Zinc gluconate is 13.4% Zn
.sup.3 Ferrous bis-glycinate (Ferrochel .RTM.) is 20.2% Fe
[0162] The dry ingredients are weighed out and added to the
deionized water with agitation. Mixing is continued until all the
ingredients are in solution. The natural flavor is then added with
agitation. The finished drink has the following attributes.
TABLE-US-00012 Green Tea Catechin Level (ppm = mg/L) 300 ppm
Turbidity 4.1 NTU pH 3.47 Mineral Levels (per 250 mL): Magnesium 80
mg = 20% RDI Zinc 3.0 mg = 20% RDI Iron 2.0 mg = 11% RDI
Carbohydrate Content (per 250 mL beverage) 15.0 g Calorie Content
(per 250 mL beverage) 60 kcal
Example 4
[0163] A calcium compatible nano-filtered green tea extract is
prepared as follows. To 100 g of a 5% w/w solution of SynerTea.TM.
green tea extract in water, 0.22 g of calcium sulfate dihydrate is
added and stirred for 15 minutes. The treated extract is heated to
168.degree. F. (75.6.degree. C.) and held for 10 minutes. The
extract is then cooled and filtered through a 0.45 micron filter.
The filtered extract thus obtained is free of insoluble calcium
components, such as oxalic acid, and does not yield sedimentation
on standing.
TABLE-US-00013 Before After Treatment Treatment Green Tea Extract
Solution pH 5.24 5.03 Green Tea Catechin Level (g per 100 g on 2.56
2.50 dry weight basis) Insoluble Calcium Components (g per 100 g on
3.16 N.D. dry weight basis) Oxalic Acid Content (g per 100 g on dry
2.62 <0.1 weight basis) N.D. = not detected
Example 5
[0164] A calcium compatible green tea extract is prepared as
follows. To 100 g of a 5% w/w solution of Plantextrakt (#285060)
Green Tea extract in water, 1.6 g of calcium chloride dihydrate is
added and stirred for 15 minutes. The treated extract is heated to
168.degree. F. (75.6.degree. C.) and held for 10 minutes. The
extract is then cooled and filtered through Whatman paper #1 and
then through a 0.45 micron filter. The filtered extract thus
obtained is free of insoluble calcium components, such as oxalic
acid and pectin, and does not yield sedimentation on standing.
TABLE-US-00014 Before After Treatment Treatment Green Tea Extract
Solution pH 5.70 5.08 Green Tea Catechin Level (g per 100 g on dry
1.50 1.60 weight basis) Insoluble Calcium Components (g per 100 g
on 4.94 N.D. dry weight basis) Oxalic Acid Content (g per 100 g on
dry weight 2.62 <0.1 basis) N.D. = not detected
Example 6
[0165] A water beverage fortified with calcium and green tea
extract is prepared according to the following formulation. Prior
to addition, an aqueous solution of the Plantextrakt green tea
extract (5% w/w) is treated to remove calcium insoluble components,
such as oxalic acid and pectin, using the procedure described in
Example 5 above.
TABLE-US-00015 Grams/ Ingredient Wt. % Liter Deionized Water 93.309
955.58 Magnesium Sulfate, anhydrous (Tangram Co.; 0.086 0.88
Holtsville, NY) .sup.1 Vitamin Premix (Roche Vitamins, Inc.; 0.029
0.30 Parsippany, New Jersey) .sup.2 Sucrose, granulated (The
Amalgamated Sugar 2.682 27.47 Co.; Ogden, Utah) Acesulfame
Potassium (Nutrinova, Inc.; 0.013 0.13 Somerset, New Jersey) Sodium
Citrate, dihydrate (A. E. Staley; 0.155 1.59 Decatur, Illinois)
Mono-potassium Phosphate (Astaris LLC; 0.086 0.88 Carteret, New
Jersey) Treated Green Tea Extract aqueous solution 2.94 30.11 from
Example 5 Citric Acid, anhydrous (A. E. Staley; 0.220 2.25 Decatur,
Illinois) Calcium gluconate (Glucona America, Inc.; 0.480 4.92
Janesville, Wisconsin) .sup.3 TOTAL = 100.0 1,024.1 .sup.1
Magnesium sulfate is 20.2% Mg .sup.2 The vitamin premix provides
the following nutrients per 250 mL serving of finished beverage:
Vitamin C 22.2 mg Niacin 2.6 mg Vitamin B6 0.26 mg Vitamin B12 0.79
.mu.g Vitamin E 3.96 International Units Zinc 1.74 mg The source of
zinc in the vitamin premix is zinc gluconate (13.4% Zn). .sup.3
Calcium gluconate is 9.31% Ca
[0166] The dry ingredients are weighed out and added to the
deionized water with agitation. The treated green tea extract
solution from Example 5 is then added and mixing is continued until
all the ingredients are in solution. The final beverage is clear
with no turbidity. The beverage has the following attributes:
TABLE-US-00016 Green Tea Catechin Level (ppm = mg/L) 227 ppm
Turbidity 30 NTU pH 3.63 Mineral Levels (per 250 mL beverage):
Magnesium 44 mg = 11.0% RDI Zinc 1.7 mg = 11.3% RDI Calcium 115 mg
= 11.5% RDI Carbohydrate Content (per 250 mL beverage) 7 g Calorie
Content (per 250 mL beverage) 28 kcal
[0167] The dimensions and values disclosed herein are not to be
understood as being strictly limited to the exact numerical values
recited. Instead, unless otherwise specified, each such dimension
is intended to mean both the recited value and a functionally
equivalent range surrounding that value. For example, a dimension
disclosed as "40 mm" is intended to mean "about 40 mm."
[0168] All documents cited in the Detailed Description of the
Invention are, in relevant part, incorporated herein by reference;
the citation of any document is not to be construed as an admission
that it is prior art with respect to the present invention. To the
extent that any meaning or definition of a term in this document
conflicts with any meaning or definition of the same term in a
document incorporated by reference, the meaning or definition
assigned to the term in this document shall govern.
[0169] While particular embodiments of the present invention have
been illustrated and described, it would be obvious to those
skilled in the art that various other changes and modifications can
be made without departing from the spirit and scope of the
invention. It is therefore intended to cover in the appended claims
all such changes and modifications that are within the scope of
this invention.
* * * * *