METHOD FOR ENHANCING REBAUDIOSIDE D SOLUBILITY IN WATER
Cross-Reference to Related Applications
[001] The present application claims priority to U.S. Serial No. 13/429,473, filed March 26,
2012, and entitled "Method for Enhancing Rebaudioside D Solubility in Water"
hereby incorporated by reference in its entirety.
Field Of Invention
[002] The present invention is directed at enhancing the solubility of Rebaudioside D in
water.
Background
[003] Sweet steviol glycoside compounds are present in small concentrations and can be
extracted from plant materials, particularly the leaves of the Stevia rebaudiana Bertoni
plant. A crude stevia extract typically comprises stevioside, steviolbioside, several
rebaudiosides, including rebaudioside A, rebaudioside B, rebaudioside C,
rebaudioside D, and rebaudioside E, and dulcoside compounds. For convenience, the
rebaudiosides may be referred to here as Reb A, Reb B, Reb C, etc.
[004] Of the Rebaudiosides, Reb A is commonly used as sweetener in beverage
applications, but has off-taste issues. Reb D has a better sugar character and more
desirable taste than Reb A, but Reb D is difficult to use in food products because of its
low solubility in water at room temperature. For instance, Reb D needs to be heated to
near boiling water temperature for 2 hours in order to achieve complete dissolution at
0.8 % concentration. At most only 300 to 450 ppm can be solubilized in water at 23
°C.
[005] Due to this low solubility, if when Reb D was is used in beverages, for example, it
was needs to be combined with other sweeteners having good solubilitythat are more
soluble in water. There is business interest now into developing sweetener
compositions higher in Reb D content, e.g., sweetener compositions having a
sweetening amount of Reb D (i.e., an amount of Reb D that perceptibly contributes to
the total sweetness provided by the sweetener), for example, sweeteners in which Reb
D is the primary sweetener. Such development is impeded, in part by the lack oflow
solubility in water of the Reb D, thus making it difficult to use in beverages, for
example. It would be advantageous, therefore, to develop improved methods to
enhance solubility of Reb D in water at room temperature (20-25 °C).
[006] Traditional processes for making beverages manufacturing process involves an
intermediate concentrated syrup step require a 6 folds concentration of ingredients in
a concentrate or syrup. This syrup is then diluted by 5 folds of with water. This works
fine if all syrup ingredients are soluble in water to the extent of 6 folds of the level in
the finished beverage. Reb D is not very soluble (about 300-450 ppm) and cannot be
provided in a syrup or concentrate in amounts sufficient enough to provide a
sweetened beverage.
[007] Accordingly, it is an object of some aspects of the present invention to provide
improved methods to enhance the solubility of Reb D in water. Additional objects
and advantages of all or certain embodiments of the systems and methods disclosed
here will be apparent to those skilled in the art given the benefit of the following
disclosure and discussion of certain exemplary embodiments.
Summary
[008] The present invention relates to enhancing the solubility of Reb D in water-based
fluids such as beverages and beverage concentrates.
[009] In one aspect, the present invention is directed to a method of enhancing the solubility
of Rebaudioside D ("Reb D") in aqueous-based liquids comprising: preparing a clear
Reb D solution by adding Reb D powder to water and heating to completely dissolve
the Reb D powder or by extracting Reb D from stevia plant using hot/boiling water,
wherein the temperature of the clear Reb D solution is above 70 °C; mixing the clear
Reb D solution with a solubility enhancer, wherein the temperature of the enhanced
Reb D solution is maintained above 70 °C, and wherein the solubility enhancer is a
water soluble organic acid or salt thereof or a hydroxyl-containing sweetener; adding
a stabilizer to the enhanced Reb D solution; wherein the stabilizer comprises a
thickener or anti-agglomeration agent; and spray drying the stabilized Reb D solution
to form a powder .
[010] In another aspect, the present invention is directed to a method of enhancing the
solubility of Rebaudioside D ("Reb D") in aqueous-based liquids comprising:
preparing a clear Reb D solution by adding Reb D powder to water and heating to
completely dissolve the Reb D powder or by extracting Reb D from stevia plant using
hot/boiling water, wherein the temperature of the clear Reb D solution is above 70 °C;
adding a stabilizer to the Reb D solution to produce a stabilized Reb D solution;
wherein the stabilizer comprises a thickener or anti-agglomeration agent; and spray
drying the stabilized Reb D solution to form a powder.
Detailed Description
[Oil] Various examples and embodiments of the inventive subject matter disclosed here are
possible and will be apparent to the person of ordinary skill in the art, given the
benefit of this disclosure. In this disclosure reference to "some embodiments,"
"certain embodiments," "certain exemplary embodiments" and similar phrases each
means that those embodiments are merely non-limiting examples of the inventive
subject matter, and there are alternative embodiments which are not excluded. Unless
otherwise indicated or unless otherwise clear from the context in which it is described,
alternative and optional elements or features in any of the disclosed embodiments and
examples are interchangeable with each other. That is, an element described in one
embodiment or example should be understood to be interchangeable or substitutable
for one or more corresponding but different elements in another described example or
embodiment and, likewise, an optional feature of one embodiment or example may
optionally also be used in other embodiments and examples. More generally, the
elements and features of any disclosed example or embodiment should be understood
to be disclosed generally for use with other aspects and other examples and
embodiments. A reference to a component or ingredient being operative or
configured to perform one or more specified functions, tasks and/or operations or the
like, is intended to mean that it can perform such function(s), task(s) and/or
operation(s) in at least certain embodiments, and may well be able to perform also one
or more other functions, tasks and/or operations.
[012] Large quantities of beverages are typically not prepared in large batches. Instead,
syrup, water, and optionally carbon dioxide are combined at the time of use or at the
time of bottling of the beverage. Traditionally one part syrup is combined with five
parts water. The syrup is a concentrate and the ingredients must be soluble in this
concentrate. For example, a typical sweetener in diet beverages is aspartame. The
aspartame must be soluble in the syrup up to 3000 ppm in order to provide the desired
sweetness value of 500 ppm when diluted with water to a final beverage. Other
sweeteners including Reb A may be used in the syrup. However, Reb D typically is
not used, or is only used as a minor component of the sweetener, because of its poor
solubility in the syrup.
[013] The present invention is directed to a method of enhancing the solubility of Reb D in
water so that the Reb D is suitable for use in concentrates or syrups. Depending on
the process used, the solubility can be increased up to 1500 ppm, or 3000 ppm, or
7000 ppm, and even up to 8000 ppm at 23 °C.
[014] First, Reb D powder is added to water and heated to completely dissolve the Reb D
powder. The concentration of the Reb D in the water is less than 3 wt %, typically
0.1 to 2.5 wt%, or 0.5 to 2.0 wt%, or 1.0 wt%.
[015] The Reb D may be added to pre-heated water, i.e. at a temperature of above 70 °C, or
the mixture of Reb D in water may be heated to a temperature of above 70 °C, to
solubilize the Reb D in the water. Typically the temperature will be 80 to 100 °C. In
either event, the heated water will solubilize the Reb D to a maximum solubility of
2.5 wt%. The resulting Reb D solution should be clear indicating that all of the Reb
D has dissolved.
[016] Alternatively, Reb D may be extracted from a stevia plant using hot/boiling water.
The temperature of the water is hot enough to extract the Reb D and at least 70 °C.
The Reb D solution is purified with techniques known in the art. The temperature of
the clear Reb D solution should remain above 70 °C.
[017] At this point, the Reb D clear solution can be spray dried resulting in fine powder.
The solubility of the Reb D increases to 1500 ppm compared to solubility of 300 ppm
for untreated Reb D.
[018] Second, the solubility is further enhanced by mixing the clear Reb D solution with a
solubilizing enhancer comprising a water soluble organic acid or salt or a hydroxylcontaining
sweetener. The concentration of solubilizing enhancer in the solution of
solubilized Reb D is 0.05% - 70% w/w.
[019] The temperature of the enhanced Reb D solution is maintained at 70 °C or above,
typically 70 to 80°C, to maintain a clear solution prior to spray drying. The enhanced
solution contains a ratio of solubilizing enhancer to Reb D from 0.01:1 to 100:1, or
0.1:1 to 50:1, or 1:1 to 20:1, for example 10:1 The pH of the solution 3 to 7.
[020] Suitable organic acids and their salts are water soluble and include sorbic acid,
ascorbic acid, benzoic acid, citric acid, tartaric acid, propionic acid, butyric acid,
acetic acid, succinic acid, glutaric acid, maleic acid, malic acid, valeric acid, caproic
acid, malonic acid, aconitic acid, potassium sorbate, sodium benzoate, sodium citrate,
amino acids, and combinations of any of them. A benefit of organic acids and salts
thereof is that they are non-nutritive and thus do not add calories to the Reb D
powder.
[021] Suitable hydroxyl-containing sweeteners are water soluble and include erythritol,
maltodextrin, sucrose, glycerol, propylene glycol, glucose, fructose, maltose,
dextrose, xylose, sorbitol, xyitol, mannitol, maltitol, lactiol, arabitol, isomalt or
combinations of any of them.
[022] In some aspects, the organic acids/salts and the sweeteners are ascorbic acid,
potassium sorbate, sodium benzoate, erythritol, maltodextrin, sucrose, or
combinations of any of them.
[023] It has been reported that the enhancement of solubility and bioavailability can be
achieved through the co-crystallization of a compound that is water insoluble with a
solubilizing enhancer. For example, the solubility and bioavailability of quercetin can
be increased 14-fold and 10-fold, respectively by co-crystallization of quercetin with
caffeine in a mass ratio of 2:1 (Adam J . Smith et al. "Mol. Pharmaceutics", 201 1, 8
(5), pp 1867-1876.) Therefore, it is believed that the water soluble organic acids/salts
and hydroxyl-containing sweeteners decrease the crystalline structure and promote the
hydration of Reb D. In addition, the organic acids/salts and hydroxyl-containing
sweeteners may form co-crystals complex with Reb D through hydrogen bonding
and/or guest-host complex resulting in increased solubility of the Reb D in water.
Finally, organic acids/salts and hydroxyl-containing sweeteners will maintain or
increase the sweetness intensity in the final beverage product. Not only can
potassium sorbate or sodium benzoate enhance the solubility of Reb D, they also acts
as preservative in finished beverage.
[024] Third, the Reb D solution is stabilized by the addition of a stabilizer in the form of a
thickener or anti-agglomeration additive such as a polysaccharide. The stabilizer can
increase spray drying efficiency, Reb D recovery, as well preventing Reb D from
crystallization when it dissolves in water. Suitable polysaccharides include gum
arabic, pectin, carrageenan, ghatti gum, acacia gum, guar gum, xanthan gum, locust
bean gum, gellen gum, agar, starch, alginate, cellulose, modified starch, carboxyl
methyl cellulose (CMC) or the combination thereof. The ratio of stabilizer to Reb D
is from 0.0 1:1 to 5:1. The stabilizer can be added as a solid or a solution.
[025] Fourth, the Reb D clear solution containing solubilizing enhancer and stabilizer is
spray dried to form a spray dried Reb D powder. Spray drying provides fine powders
with large surface area.
[026] The spray dried Reb D powder has a solubility of up to 8000 ppm at 23 °C. This Reb
D powder may be added to beverage concentrates at amounts of at least 1200 ppm
and up to 5000 ppm, typically 1800 to 3000 ppm, at room temperature (20-25 °C).
[027] The resulting Reb D powder containing the organic acids or salts thereof or the
hydroxyl-containing sweetener dissolves in water rapidly with minimal mixing
energy. Beverages made with modified Reb D powder have a comparable taste profile
to beverages made with untreated Reb D. That is, the treated Reb D powder
maintains the sweetness characteristics of the untreated Reb D. Further, not only do
the sugar alcohols enhance the solubility of Reb D, but can also increase sweetness
over all.
[028] In accordance with another aspect of the present invention, the solubility of the Reb D
can be increased upwards to 1500 ppm at 23 °C. This aspect is similar to the aspect
described above, but without the addition of solubilizing enhancer.
[029] First, Reb D powder is added to water and heated to completely dissolve the Reb D
powder. The concentration of the Reb D in the water is less than 2.5 wt. %, typically
0.1 to 2.5 wt%, or 0.5 to 2.0 wt%, or 1.0 wt%.
[030] The Reb D may be added to pre-heated water, i.e. at a temperature of above 70 °C, or
the mixture of Reb D in water may be heated to a temperature of above 70 °C, to
solubilize the Reb D in the water. Typically the temperature will be 80 to 100 °C. In
either event, the heated water will solubilize the Reb D to a maximum solubility of
2.5 wt%. The resulting Reb D solution should be clear indicating that all of the Reb
D has dissolved.
[031] Alternatively, Reb D may be extracted from a stevia plant using hot/boiling water.
The temperature of the water is hot enough to extract the Reb D and at least 70 °C.
The Reb D solution is purified with techniques known in the art. The temperature of
the clear Reb D solution should remain above 70 °C.
[032] At this point, the Reb D clear solution can be spray dried resulting in fine powder.
The solubility of the Reb D increases to 1500 ppm compared to that of 300 ppm of
untreated Reb D.
[033] Second, the Reb D solution is stabilized by the addition of a stabilizer in the form of a
thickener or anti-agglomeration additive such as a polysaccharide. Suitable
polysaccharides include gellan gum, gum Arabic, pectin, carrageenan, ghatti gum,
acacia gum, guar gum, xanthan gum, locust bean gum, agar, starch, alginate,
cellulose, modified starch, carboxyl methyl cellulose (CMC) or the combination
thereof.
[034] The temperature of the Reb D solution is maintained above 70 °C, typically 70 to
80°C, to maintain a clear solution prior to spray drying.
[035] Third, the stabilized Reb D solution containing a solubilizing enhancer is spray dried
to form a spray dried Reb D powder. Spray drying provides fine powders which
provide a large surface area. Fine particle sizes are generally 1 to 300 microns. The
finer the particle size, the greater the total surface area, and the greater the dissolution
rate when the powder is added to the concentrate.
[036] The spray dried Reb D powder has a solubility of up to 3000 ppm at 23 °C. This Reb
D powder may be added to beverage concentrates at amounts of at least 1200 ppm
and up to 3000 ppm, typically 1800 to 3000 ppm, at room temperature.
[037] The resulting Reb D solution dissolves in water rapidly with minimal mixing energy.
Beverages made with stabilized Reb D powder have a comparable taste profile to
beverages made with untreated Reb D. That is, the stabilized Reb D powder
maintains the sweetness characteristics of the untreated Reb D.
[038] Beverages prepared with the Reb D powder in accordance with either aspect
discussed above, are stable at pH 3 to 5 and are clear with no settling, precipitation,
and color change observed over time.
[039] Reb D is obtained from the stevia plant in any suitable manner. For example, the Reb
D may be extracted with hot/boiling water or water/ethanol mixture. The Reb D is
isolated and purified. As noted above, this solution can be spray dried resulting in
increased solubility.
[040] The spray drying may be by any suitable method with any suitable equipment. Buchi
mini spray dryer is used to produce Reb D powder. The machine conditions are as
follows: Evaporative capacity: 1.0 L/hr water; Air flow: max of 35 cu. m/hr;
Maximum temperature input: 220 C; Spray gas and pressure: compressed air or
nitrogen, 200-1000 l/hr, 5-8 bar; Nozzle diameter: 0.7 mm.
[041] The Reb D powder prepared in accordance with embodiments herein may be used in
beverage products including, ready to drink liquid formulations, beverage
concentrates and the like. The Reb D is particularly useful for beverage concentrates
or syrups where much higher amounts of sweetener are needed in solution.
[042] Beverages include, e.g., carbonated and non-carbonated soft drinks, fountain
beverages, frozen ready-to-drink beverages, coffee beverages, tea beverages, dairy
beverages, powdered soft drinks, as well as liquid concentrates, flavored waters,
enhanced waters, fruit juice and fruit juice-flavored drinks, sport drinks, and alcoholic
products.
[043] The terms "beverage concentrate" and "syrup" are used interchangeably throughout
this disclosure. At least certain exemplary embodiments of the beverage concentrates
contemplated are prepared with an initial volume of water to which the additional
ingredients are added. Full strength beverage compositions may be formed from the
beverage concentrate by adding further volumes of water to the concentrate.
Typically, for example, full strength beverages may be prepared from the concentrates
by combining approximately 1 part concentrate with between approximately 3 to
approximately 7 parts water. In certain exemplary embodiments the full strength
beverage is prepared by combining 1 part concentrate with 5 parts water. In certain
exemplary embodiments the additional water used to form the full strength beverages
is carbonated water. In certain other embodiments, a full strength beverage is directly
prepared without the formation of a concentrate and subsequent dilution.
[044] Water is a basic ingredient in the beverage products disclosed here, typically being the
vehicle or primary liquid portion in which the remaining ingredients are dissolved,
emulsified, suspended or dispersed. Purified water can be used in the manufacture of
certain embodiments of the beverages disclosed here, and water of a standard
beverage quality can be employed in order not to adversely affect beverage taste,
odor, or appearance. The water typically will be clear, colorless, free from
objectionable minerals, tastes and odors, free from organic matter, low in alkalinity
and of acceptable microbiological quality based on industry and government
standards applicable at the time of producing the beverage. In certain typical
embodiments, water is present at a level of from about 80% to about 99.9% by weight
of the beverage. In at least certain exemplary embodiments the water used in
beverages and concentrates disclosed here is "treated water," which refers to water
that has been treated to reduce the total dissolved solids of the water prior to optional
supplementation, e.g., with calcium as disclosed in U.S. Patent No. 7,052,725.
Methods of producing treated water are known to those of ordinary skill in the art and
include deionization, distillation, filtration and reverse osmosis ("r-o"), among others.
The terms "treated water," "purified water,", "demineralized water," "distilled water,"
and "r-o water" are understood to be generally synonymous in this discussion,
referring to water from which substantially all mineral content has been removed,
typically containing no more than about 500 ppm total dissolved solids, e.g. 250 ppm
total dissolved solids.
[045] Notwithstanding the claims, the invention is also defined by way of the following
clauses:
1. A method of enhancing the solubility of Rebaudioside D ("Reb D") in
aqueous-based liquids comprising:
a . preparing a clear Reb D solution by adding Reb D powder to water and
heating to completely dissolve the Reb D powder, or by extracting Reb D from
stevia plant using hot/boiling water or water/ethanol, wherein the temperature
of the clear Reb D solution is above 70 °C;
b. mixing the clear Reb D solution with a solubilizing enhancer, wherein the
temperature of the enhanced Reb D solution is maintained above 70 °C, and
wherein the solubilizing enhancer is a water soluble organic acid salt, a water
soluble organic acid, or a hydroxyl-containing sweetener;
c . adding a stabilizer to the enhanced Reb D solution to produce a stabilized Reb
D solution; wherein the stabilizer comprises a thickener or anti-agglomeration
agent; and
d. spray drying the stabilized Reb D solution to form a powder.
2. The method according to clause 1 wherein the concentration of Reb D in the
clear Reb D solution in step (a) 0.05 wt% to 2.5 wt%.
3. The method according to any of the preceding clauses comprising adding Reb
D powder to water at a temperature of above 70 °C or adding the Reb D powder to
water and then heating to a temperature of above 70 °C.
4. The method according to any of the preceding clauses wherein the temperature
in step (a) is 80 to 100 °C.
5. The method according to any of the preceding clauses wherein the ratio of the
hydroxyl-containing sweetener to Reb D is from 0.01:1 to 100:1.
6. The method according to any of the clauses 1-4 wherein the ratio of hydroxylcontaining
sweetener to Reb D is from 0.1:1 to 50: 1.
7. The method according to any of the clauses 1-4 wherein the ratio of stabilizer
to Reb D is from 0.01 :1 to 5:1.
8. The method according to any of the preceding clauses wherein the enhanced
Reb D solution is maintained above 70 °C to maintain a clear solution.
9. The method according to any of the preceding clauses wherein the solubilizing
enhancer is an acid salt or an organic acid selected from the group consisting of
potassium sorbate, sodium benzoate, sodium citrate, sorbic acid, ascorbic acid,
benzoic acid, citric acid, tartaric acid, propionic acid, butyric acid, succinic acid,
glutaric acid, maleic acid, malic acid, valeric acid, caproic acid and amino acids.
10. The method of claim 9 wherein the organic acid salt or the organic acid is
potassium sorbate, sodium benzoate, or ascorbic acid.
11. The method according to any of clauses 1-8 wherein the solubilizing enhancer
is a hydroxyl-containing sweetener selected from the group consisting of erythritol,
sucrose, maltodextrin, glycerol, propylene glycol, glucose, fructose, maltose,
dextrose, xylose, sorbitol, xyitol, mannitol, maltitol, lactiol, arabitol, isomalt, or
mixtures of any of them.
12. The method of claim 11 wherein the hydroxyl-containing sweetener is
sucrose, maltodextrin, erythritol, or a combination thereof.
13. The method according to any of the preceding clauses wherein the stabilizer is
selected from the group consisting of gum Arabic, pectin, carrageenan, ghatti gum,
acacia gum, guar gum, xanthan gum, gellan gum, locust bean gum, agar, starch,
alginate, cellulose, modified starch, carboxyl methyl cellulose (CMC) or mixtures of
any of them.
14. The method according to any of the preceding clauses wherein the stabilized
solution is maintained above 70 °C to maintain a clear solution.
15. The method according to any of the preceding clauses wherein the spray dried
powder has a particle size of 1 to 300 microns.
16. The method according to any of the preceding clauses wherein the spray dried
powder has a solubility of up to 8000 ppm at 23 °C.
17. The method according to any of the preceding clauses wherein the stabilizer is
gum arabic.
18. A beverage comprising the powder prepared in accordance with any of the
preceding clauses.
19. A beverage concentrate comprising the powder prepared in accordance with
any of the preceding clauses.
[046] EXAMPLES
[047] Example 1
[048] To a 1000 ml beaker, 3 g Reb D and 600 g water were added. The Reb D mixture was
heated to 80-100 °C until completely dissolved. The temperature was maintained
above 70 °C to keep Reb D clear solution. Subsequently, the Reb D clear solution
was subjected to spray drying resulting in powder containing 95% Reb D.
[049] Example 2
[050] To a 1000 ml beaker, 3 g Reb D and 580 g water were added. The Reb D mixture was
heated to 80-100 °C until completely dissolved. Then, 6 g (25%) gum arabic solution
were added. The temperature was maintained above 70 °C to keep Reb D clear
solution. Subsequently, the Reb D clear solution was subjected to spray drying
resulting in powder containing 66.67% Reb D.
[051] Example 3
[052] To a 1000 ml beaker, 3 g Reb D and 580 g water were added. The Reb D mixture was
heated to 80-100 °C until completely dissolved. Then, 9 g sucrose and 6 g (25%) gum
arabic were added. The temperature was maintained above 70 °C to keep Reb D clear
solution. Subsequently, the Reb D clear solution was subjected to spray drying
resulting in powder containing 22.2% Reb D.
[053] Example 4
[054] To a 1000 ml beaker, 3 g Reb D and 580 g water were added. The Reb D mixture was
heated to 80-100 °C until completely dissolved. Then, 9 g maltodextrin, 3 g erythritol,
and 6 g (25%) gum arabic were added. The temperature was maintained above 70 °C
to keep Reb D clear solution. Subsequently, the Reb D clear solution was subjected
to spray drying resulting in powder containing 18.18% Reb D.
[055] Example 5
[056] To a 1000 ml beaker, 3 g Reb D and 580 g water were added. The Reb D mixture was
heated to 80-100 °C until completely dissolved. Then, 3 g maltodextrin, 3 g erythritol,
and 6 g (25%) gum arabic were added. The temperature was maintained above 70 °C
to keep Reb D clear solution. Subsequently, the Reb D clear solution was subjected
to spray drying resulting in powder containing 28.57% Reb D.
[057] Example 6
[058] To a 1000 ml beaker, 3 g Reb D and 580 g water were added. The Reb D mixture was
heated to 80-100 °C until completely dissolved. Then, 6 g maltodextrin, 3 g erythritol,
and 12 g (25%) gum arabic were added. The temperature was maintained above 70 °C
to keep Reb D clear solution. Subsequently, the Reb D clear solution was subjected
to spray drying resulting in powder containing 20%> Reb D.
[059] Example 7
[060] To a 1000 ml beaker, 3 g Reb D and 580 g water were added. The Reb D mixture was
heated to 80-100 °C until completely dissolved. Then, 9 g maltodextrin and 6 g (25%)
gum arabic solution were added. The temperature was maintained above 70 °C to
keep Reb D clear solution. Subsequently, the Reb D clear solution was subjected to
spray drying resulting in powder containing 22.2% Reb D.
[061] Example 8
[062] To a 1000 ml beaker, 3 g Reb D and 550 g water were added. The Reb D mixture was
heated to 80-100 °C until completely dissolved. Then, 30 g maltodextrin, 24 g
erythritol, and 12 g (25%) gum arabic were added. The temperature was maintained
above 70 °C to keep Reb D clear solution. Subsequently, the Reb D clear solution
was subjected to spray drying resulting in powder containing 5% Reb D.
[063] Example 9
[064] To a 1000 ml beaker, 3 g Reb D and 800 g water were added. The Reb D mixture was
heated to 80-100 °C until completely dissolved. Then, 24 g (25%) gum arabic solution
was added. The temperature was maintained above 70 °C to keep Reb D clear
solution. Subsequently, the Reb D clear solution was subjected to spray drying
resulting in powder containing 33.3% Reb D.
[065] Example 10
[066] To a 1000 ml beaker, 3 g Reb D and 516 g water were added. The Reb D mixture was
heated to 80-100 °C until completely dissolved. Then, 60 g maltodextrin and 24 g
(25%) gum arabic solution were added. The temperature was maintained above 70 °C
to keep Reb D clear solution. Subsequently, the Reb D clear solution was subjected
to spray drying resulting in powder containing 4.35% Reb D.
[067] Example 11
[068] To a 1000 ml beaker, 3 g Reb D and 580 g water were added. The Reb D mixture was
heated to 80-100 °C until completely dissolved. Then, 45 g maltodextrin and 24g
(25%) gum arabic solution were added. The temperature was maintained above 70 °C
to keep Reb D clear solution. Subsequently, the Reb D clear solution was subjected
to spray drying resulting in powder containing 5.56% Reb D.
[069] Example 12
[070] To a 1000 ml beaker, 3 g Reb D and 580 g water were added. The Reb D mixture was
heated to 80-100 °C until completely dissolved. Then, 30 g maltodextrin and 24g
(25%>) gum arabic solution were added. The temperature was maintained above 70 °C
to keep Reb D clear solution. Subsequently, the Reb D clear solution was subjected
to spray drying resulting in powder containing 7.69% Reb D.
[071] Example 13
[072] To a 1000 ml beaker, 1.5 g Reb D and 500 g water were added. The Reb D mixture
was heated to 80-100 °C until completely dissolved. Then, 30 g erythritol was added.
The temperature was maintained above 70 °C to keep Reb D clear solution.
Subsequently, the Reb D clear solution was subjected to spray drying resulting in
powder containing 4.76% Reb D.
[073] Example 14
[074] To a 2000 ml beaker, 5 g Reb D and 995 g water were added. The Reb D mixture was
heated to 80-100 °C until completely dissolved. Then, 5 g sucrose was added. The
temperature was maintained above 70 °C to keep Reb D clear solution. Subsequently,
the Reb D clear solution was subjected to spray drying resulting in powder containing
47.5% Reb D.
[075] Example 15
[076] To a 2000 ml beaker, 5 g Reb D and 995 g water were added. The Reb D mixture was
heated to 80-100 °C until completely dissolved. Then, 2.5 g sucrose was added. The
temperature was maintained above 70 °C to keep Reb D clear solution. Subsequently,
the Reb D clear solution was subjected to spray drying resulting in powder containing
63.3% Reb D.
[077] Example 16
[078] To a 1000 ml beaker 5 g Reb D (95%) and 980 g water were added. The Reb D
mixture was heated to 80-100 °C until completely dissolved. Then, 10 g glucose was
added. The temperature was maintained above 70 °C to keep Reb D clear solution.
Subsequently, the Reb D clear solution was subjected to spray drying resulting in
powder containing 3 1.67% Reb D.
[079] Example 17
[080] To a 1000 ml beaker 5 g Reb D (95%) and 980 g water were added. The Reb D
mixture was heated to 80-100 °C until completely dissolved. Then, 10 g potassium
sorbate was added. The temperature was maintained above 70 °C to keep Reb D clear
solution. Subsequently, the Reb D clear solution was subjected to spray drying
resulting in powder containing 3 1.67% Reb D.
[081] Example 18
[082] To a 1000 ml beaker 5 g Reb D (95%) and 980 g water were added. The Reb D
mixture was heated to 80-100 °C until completely dissolved. Then, 10 g sodium
benzoate was added. The temperature was maintained above 70 °C to keep Reb D
clear solution. Subsequently, the Reb D clear solution was subjected to spray drying
resulting in powder containing 3 1.67% Reb D.
Table 1. Modified Reb D Solubility in Water
] As used in this disclosure, unless otherwise specified, the term "added" or
"combined" and like terms means that the multiple ingredients or components
referred to (e.g., one or more solubility enhancer, polysaccharide, etc.) are combined
in any manner and in any order, with or without stirring or the like, etc. For example,
one or more ingredients can be dissolved into one or more other ingredients, or
sprayed together, etc. As used here, a slurry, may be a suspension, dispersion, or
other form of flowable material.
While this disclosure mentions specific examples and embodiments, those skilled in
the art will appreciate that there are numerous variations and modifications within the
spirit and scope of the invention as set forth in the appended claims. Each word and
phrase used in the claims is intended to include all its dictionary meanings consistent
with its usage in this disclosure and/or with its technical and industry usage in any
relevant technology area. Indefinite articles, such as "a," and "an" and the definite
article "the" and other such words and phrases are used in the claims in the usual and
traditional way in patents, to mean "at least one" or "one or more." The word
"comprising" is used in the claims to have its traditional, open-ended meaning, that is,
to mean that the product or process defined by the claim may optionally also have
additional features, elements, etc. beyond those expressly recited in the claim.
What is Claimed is:
1. A method of enhancing the solubility of Rebaudioside D ("Reb D") in aqueous-based
liquids comprising:
a . preparing a clear Reb D solution by adding Reb D powder to water and
heating to completely dissolve the Reb D powder, or by extracting Reb D from
stevia plant using hot/boiling water or water/ethanol, wherein the temperature
of the clear Reb D solution is above 70 °C;
b. mixing the clear Reb D solution with a solubilizing enhancer, wherein the
temperature of the enhanced Reb D solution is maintained above 70 °C, and
wherein the solubilizing enhancer is a water soluble organic acid salt, a water
soluble organic acid, or a hydroxyl-containing sweetener;
c . adding a stabilizer to the enhanced Reb D solution to produce a stabilized Reb
D solution; wherein the stabilizer comprises a thickener or anti-agglomeration
agent; and
d. spray drying the stabilized Reb D solution to form a powder.
2. The method according to claim 1 wherein the concentration of Reb D in the clear Reb
D solution in step (a) 0.05 wt% to 2.5 wt%.
3. The method according to claim 1 adding Reb D powder to water at a temperature of
above 70 °C or adding the Reb D powder to water and then heating to a temperature
of above 70 °C.
4. The method according to claim 1 wherein the temperature in step (a) is 80 to 100 °C.
5. The method according to claim 1 wherein the enhanced Reb D solution is maintained
above 70 °C to maintain a clear solution.
6. The method according to claim 1 wherein the stabilized solution is maintained above
70 °C to maintain a clear solution.
7. The method according to claim 1 wherein the ratio of the hydroxyl-containing
sweetener to Reb D is from 0.01 :1 to 100: 1
8. The method according to claim 1 wherein the ratio of hydroxyl-containing sweetener
to Reb D is from 0.1:1 to 50: 1
9. The method according to claim 1 wherein the ratio of stabilizer to Reb D is from
0.01:1 to 5:1.
10. The method according to claim 1 wherein the solubilizing enhancer is an acid salt or
an organic acid selected from the group consisting of potassium sorbate, sodium
benzoate, sodium citrate, sorbic acid, ascorbic acid, benzoic acid, citric acid, tartaric
acid, propionic acid, butyric acid, succinic acid, glutaric acid, maleic acid, malic acid,
valeric acid, caproic acid and amino acids.
11. The method of claim 10 wherein the organic acid salt or the organic acid is potassium
sorbate, sodium benzoate, or ascorbic acid.
12. The method according to claim 1 wherein the solubilizing enhancer is a hydroxylcontaining
sweetener is selected from the group consisting of erythritol, sucrose,
maltodextrin, glycerol, propylene glycol, glucose, fructose, maltose, dextrose, xylose,
sorbitol, xyitol, mannitol, maltitol, lactiol, arabitol, isomalt, or mixtures of any of
them.
13. The method of claim 12 wherein the hydroxyl-containing sweetener is sucrose,
maltodextrin, erythritol, or a combination thereof.
14. The method according to claim 1 wherein the stabilizer is selected from the group
consisting of gum Arabic, pectin, carrageenan, ghatti gum, acacia gum, guar gum,
xanthan gum, gellan gum, locust bean gum, agar, starch, alginate, cellulose, modified
starch, carboxyl methyl cellulose (CMC) or mixtures of any of them.
15. The method according to claim 1 wherein the spray dried powder has a particle size of
1 to 300 microns.
16. The method according to claim 1 wherein the spray dried powder has a solubility of
up to 8000 ppm at 23 °C.
17. The method of claim 1 wherein the stabilizer is gum arabic.
18. A beverage comprising the powder prepared in accordance with claim 1.
19. A beverage concentrate comprising the powder prepared in accordance with claim 1.