STABILIZING SORBIC ACID OR BENZOIC ACID IN SYRUPS
AND FINISHED BEVERAGES
FIELD OF THE INVENTION
[001] The invention relates to a method for stabilizing sorbic acid or benzoic acid in syrup
and finished beverages.
BACKGROUND OF THE INVENTION
[002] Sorbic acid (2,4,-hexadienic acid) is widely used as a preservative in foods and
beverages. A common problem when using sorbic acid in beverage applications is
low solubility in syrups and finished beverages
[003] Because of its low solubility, sorbic acid is unstable in syrups and finished beverages
resulting in creaming and precipitates. For example, the solubility of sorbic acid in
water at roo temperature is 0.16 w . The solubility of sorbic acid in a solution
containing 60 wt% sugar is 0.08 wt%. The solubility of sorbic acid i high acid
syrup is less than 0.1 wt%.
[004] It is desired to have at least 1200-1600 ppra sorbic acid in syrups and at least 200-
250 ppm in finished beverages, but such amounts have been difficult to achieve due
to low solubility, creaming, settling, precipitation, and phase separation.
[005] Likewise benzoic acid is a widely used preservative but also has low solubility in
concentrated syrup and finished beverage; thus it is also desired to increase the
solubility of benzoic acid in syrups and finished beverages.
BRIEF SUMMARY OF THE INVENTION
[006] An aspect of the invention relates to a method of preparing a sorbic acid microdispersion
by solubilizing a salt of sorbic acid, in particular potassium sorbate, in
water to form a potassium sorbate solution, adding a stabilizer with water to for a
stabilizer solution; combining the potassium sorbate solution and stabilizer solution
and mixing; and adjusting the pH to form a stabilized sorbic acid dispersion, wherein
the viscosity of the dispersion is no greater than 1000 cps.
[007] Another aspect relates to a method of making beverage syrup by adding the sorbic
acid micro-dispersion described above to beverage syrup.
[008] Another aspect relates to a method of making a soft drink beverage by adding
carbonated water or treated water to the concentrated beverage syrup described
above
[009] A further aspect of the invention relates to a method of preparing a benzoic acid
micro-dispersion by solubilizing a salt of benzoic acid, in particular sodium benzoate
or potassium benzoate, in water to form a sodium benzoate solution, adding a
stabilizer with water to form a stabilizer solution; combining the sodium benzoate
solution and stabilizer solution and mixing; and adjusting the pH to form a stabilized
benzoic acid dispersion, wherein the viscosity of the dispersion is no greater than
000 cps.
[010] Another aspect relates to a method of making beverage syrup by adding the benzoic
acid micro-dispersion described above to beverage syrup.
[011] Another aspect relates to a method of making a soft drink beverage by adding
carbonated water or treated water to the beverage syrup described above.
BRIEF DESCRIPTION OF THE DRAWINGS
[012] Fig. 1 depicts sorbic acid dispersion viscosity vs. temperature for a sorbic acid
dispersion prepared in accordance with aspects of the presen invention.
[013] Fig. 2 depicts sorbic acid dispersion viscosity vs. % of gum arable for a sorbic acid
dispersion prepared in accordance with aspects of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
. ? _
[014] Aspects of the invention relate to a method for stabilizing sorbic acid or benzoic acid
in syrup and finished beverages. A stabilizer is employed to stabilize the sorbic acid
or benzoic acid as well as to maintain a low viscosity.
[015] A micro-dispersion is formed with sorbic acid or benzoic acid and a stabilizer such
as gum arable. The stabilized sorbic acid or benzoic acid micro-dispersion is shelf
stable and has low viscosity of less than 200 cPs, in particular less than 100 cPs as
measured by Brookfield viscometer at 25 °C. Concentrated syrups and finished
beverages containing the stabilized sorbic acid or benzoic acid micro-dispersion are
likewise shelf stable.
[016] In the context of the present application, a beverage or concentrated syrup is stable if
there is no creaming, settling, precipilation, or phase separation observed for at least
40 days at 35 to 110 °F, in particular at 40 to 90 ° .
[0 ] A micro-dispersion means that sorbic acid or benzoic- acid particles are present in the
size of 0.1 to 50 microns, for example 0.5 to 10 microns.
[018] In further aspects, the micro-dispersion may contain both sorbic acid and benzoic
ac d particles. In addition, the micro-dispersion is compatible with other
preservatives such as, but not limited to, sodium hexametaphosphate,
calcium/sodium (Ca/Na EDTA), and lauroyl arginine ethyl ester (LAE) in addition to
the sorbic acid and benzoic acid particles.
[019] The method of the invention wi l be discussed initially n relation to stabilizing
sorbic acid, but unless otherwise specified, stabilizing benzoic acid will contain the
same method steps and parameters.
[020] Aspects of the invention relate to a method of preparing the sorbic acid microdispersions
in accordance with the following steps:
[021] Potassium sorbate is solubilized in water to form a potassium sorbate solution.
Potassium sorbate is readily soluble in water, e.g. 45 wt% in water at room
temperature. The concentration of potassium sorbate in water is in the range of 30-
65 w %. The temperature of the water in the solution is 20 to 00 °C, or example 20
to 80 °C, or 25 to 60 °C, or 45 to 60 °C.
[022] A stabilizer solution is formed by dissolving or dispersing a stabilizer in water. The
stabilizer is present in the stabilizer solution in an amount of 0.1 to 40 t%, for
example 0.5 to 30 wt%. The temperature of the water is 30 to 60 °C and may be the
same or different from the temperature of the potassium sorbate solution.
[023] The potassium sorbate solution is combined with the stabilizer solution under high
shear mixing at 3000-10000 rpm wherein the pH is maintained at 3 to 5 to convert all
sorbate to sorbic acid and form the micro-dispersion. The temperature of the
combined solutions remains between 20-60 C, for example 40-50 °C.
[024] The resulting amount of sorbic acid in dispersion is in the range of 1-30 w w, for
example 3-20 w/w. The dispersion contains 0.1-25 wt%, for example 0 3-20 wr
stabilizer and 3 to 20 wt% sorbic acid.
[025] Th sorbic acid dispersion is further mixed under high shear mixing for 5 minutes. If
necessary, the pH of the dispersion is adjusted to 2.5 to 4, for example 2.8 to 3.5, byadding
a food grace acid. The acid is added in an amount to achieve the desired pH
and is well within the skill of the art. The dispersion of sorbic acid and gum arable is
more stable (less settling) at H levels of 2.8-3.5. As pH is increased, the dispersion
viscosity increases.
[026] To reduce the particle size, the sorbic acid dispersion further undergoes
homo ge zation at 3000-5000 psi for 1-2 pass resulting homogeneous, fine
dispersion. The particle size in the dispersion, for example to a particle size of 0 1 to
5 microns. The viscosity of the dispersion is less than 200 cPs as measured by
Brookfield viscometer at 25 °C.
[027] The stability of sorbic acid is related to the level of stabilizer. For example, the
dispersion settles at 5-10% sorbic acid solid when the amount of gum arable is less
than 8 wt%. The stability of sorbic acid dispersion depends on the viscosity. The
dispersion stability increases as viscosity increases. As shown in the examples, the
dispersion is stable with no creaming, settling, precipitation, or phase separation
when dispersion contains 0.1-20 wt% stabilizers and 5- 5 wt% sorbic acid
[028] For example, a stable sorbic acid dispersion is obtained when carboxymethyl
cellulose (CMC) is used as a stabilizer. The level of CMC in the dispersion is in the
range of 0.1-3% w/w depending on the molecular weight of CMC. The viscosity of
the dispersion with CMC is in the range of 10- 000 cPs for example 25-100 cPs.
[029] The dispersion is added into syrup to provide a concentration of 0 .12-0.5 wt% (1200-
5000 ppm) sorbic acid in the syrup. The syrup is mixed thoroughly by any suitable
method such as mechanical mixing. The syrup containing the sorbic acid dispersion
is stable and homogeneous. The sorbic acid dispersion syrup is instantly soluble
when it is diluted into carbonated water resulting in clear softer beverage.
[030] The resulting CSD beverage contains 200-800 ppm, for example, 250-650 ppm,
sorbic acid. I one example, the finished CSD beverage contains 250 ppm sorbic
acid. The resulting beverage is stable.
[031] In a similar way, shelf stable benzoic acid dispersion is prepared. Sodium or
potassium benzoate is soiubilized in water to form a sodium or potassium benzoate
solution. Sodium benzoate is readily soluble in water, e.g. 30 wt% in water at room
temperature. Likewise, potassium benzoate is readily soluble in water, e.g. 39 wt%
in water at room temperature. The concentration of sodium or potassium benzoate in
water is in the range of 30-65 wt% at temperature between 20-70 °C. The
temperature of the water in the solution is 20 to 100 °C, for example 20 to 80 °C, or
25 to 60 °C, or 45 to 60 °C.
[032] A stabilizer solution is formed by dissolving or dispersing a stabilizer in water. The
stabilizer is present in the stabilizer solution in an amount of 0.1 to 40 wt¾, for
example 0.5 to 30 wt%. The pH of the stabilizer-containing solution is kept at 2.5-4.
The temperature of the water is 30 to 60 °C and may be the same or different from
the temperature of the sodium or potassium benzoate solution.
[033 The sodium or potassium benzoate solution is combined with the stabilizer solution
under high shear mixing at 3000-10000 rpm wherein the p is maintained at 2 5 to 5
to convert al benzoate to benzoic acid and form the micro-dispersion. The
temperature of the combined solutions remains between 20-60 °C, for example 40
°C.
[034] The resulting amount of benzoic acid in dispersion is in the range of 1-30 w/w, for
example 5-10 w/w. The dispersion contains 0.1-25 wi%, for example 0.3-20 wt%,
stabilizer and 5-20 wt% benzoic acid.
[035] The benzoic acid dispersion is further mixed under high shear mixing for 2 to 5
minutes, for example 5 minutes. The final dispersion pH is adjusted from between
2.5 to 4 using any suitable food grade acid as discussed above. The stability of
benzoic acid dispersion depends on the viscosity. The dispersion stability increase as
increasing viscosity.
[036] For example, stable benzoic acid dispersions are obtained when carboxymethyl
cellulose (CMC) is used as a stabilizer. The level of CMC in the dispersion is in the
range of 0.1-3% w/w depending on the molecular weight of the CMC. The viscosity
of benzoic acid dispersion with CMC is in the range of 10-1000 cPs. for example 25-
100 cps.
[037] Benzoic acid dispersion is added into syrup in a concentration of 0.1-0.5 w/t%. The
syrup of pH is adjusted to pH 2.5-4 with a suitable food grade acid.
[038] The syrup containing the benzoic acid dispersion is stable and homogeneous. The
benzoic acid dispersion syrup is instantly soluble when it is diluted into carbonated
water or treated water resulting in clear softer beverage.
[039] The resulting beverage contains 200-800 ppra, for example, 250-500 ppm, benzoic
acid. n one example, the finished beverage contains 250 ppm benzoic acid. The
resulting beverage is stable.
[040] The water suitable with any aspect of the invention may be treated to reduce the total
dissolved solids of the water. 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
[041] The stabilizer suitable with any aspect of the invention may be any suitable
biopolymer or a modified polysaccharide such as gum arabic, carboxymethyl
cellulose (CMC), gellan gum, pectin, earrageenan, ghatti gum, guar gum, xanthan
gum, locust gum, agar, starch, alginate, cellulose, modified starch, or any
combination thereof. Suitable gums generally have a molecular weight of 10,000 to
,000,000 Daiions. For example, such stabilizers reduce sorbic acid particle size,
increase dispersion stability by electrostatic and steric repulsion, and prevent sorbic
aid from crystallization aggregation, and flocculation.
[042] The food grade acid suitable with any aspect of the invention may be any suitable
acid such as citric acid, phosphoric acid, tartaric acid, maleic acid, or glutaric acid.
Typically, citric acid or phosphoric acid is used
[043] T re beverage syrup suitable with any aspect of the invention may be any suitable
beverage syrup suitable for carbonated soft drinks. Such syrups typically contain
sugar in concentrations of 40 w/w% to 70 w/w for example, cane sugar or HFCS.
Alternatively the syrups may be of the '"diet" soda variety with non-nutritive
sweeteners such as, but not limited to, acesulfame potassium, aspartame, sacchar in
sucralose, neotame, monatin, sodium cyclamate, and steviol glycosides. Other
ingredients include flavorants such as cola or citrus flavors and colorants, food acids
such as citric acid, vitamins, preservative cocktail, and caffeine.
[044] Typically a beverage is formed by combining 1 part syrup with 3-7 parts water, most
typically 1 part syrup to 5 parts water (called a 1:5 throw). A typical non-nutritive
beverage is formed by combining 1 part non-nutritive syrup with 30-50 parts water.
In forming carbonated soft drinks (CSDs), the syrup is diluted with treated
carbonated water.
[045] The dispersion is pumpable so it may be used in fountain dispensers. Hence, at the
fountain dispenser, the syrup is combined with the carbonated water to form the
beverage for immediate consumption.
[046] Notwithstanding the claims, the invention is also defined by way of the following
clauses:
[047] Clause : A method of preparing a stabilized micro-dispersion comprising
a . solubilizing a sorbate or benzoate in water to form a sorbate or benzoate
solution, wherein the temperature of the water is 20 to 100 °C;
b. combining a stabilizer with water to form a stabilizer solution, wherein the
stabilizer is a biopolymer or a modified polysaccharide:
c . combining the sorbate or benzoate solution an stabilizer solution and mixing
to form a sorbic acid or benzoic acid micro-dispersion comprising 0 . 1 to 25
wt% stabilizer and 1 to 30 wt% sorbic acid or benzoic acid, each based on
total weight of the micro-dispersion; and
d. adjusting the pH of the micro-dispersion to 2.5 to 4, wherein the viscosity of
the dispersion is no greater than 1000 cPs at 25 °C.
[048] Clause 2 : The method of clause 1 wherein the viscosity of the micro-dispersion is
no greater than 00 cPs at 25 °C.
[049] Clause 3: The method of clause 1 or clause 2 wherein the micro-dispersion comprises
1 to 3 wt% stabilizer based on total weight of the micro-dispersion.
[050] Clause 4 ; The method of any of clauses 1-3 wherein the micro-dispersion comprises
5 to wt% sorbic acid or benzoic acid, each based on total weight of the microdispersion.
[051 Clause 5 : The method of any of clauses 1-4 comprising in a . solubilizing potassium
sorbate to form solution comprising 30-65 wt% potassium sorbate.
[052] Clause 6 ; The method of any of clauses 1-4 comprising in a . solubilizing sodium or
potassium benzoate to form a sodium or potassium benzoate solution to form a
benzoate solution comprising 30-65 t% sodium or potassium benzoate.
[053] Clause 7: The method of any of clauses 1-6 wherein, in step a, the temperature of the
water is 20 to 70 C
[054] Clause 8 ; The method of any of clauses 1-7 wherein the stabilizer is selected from
the group consisting of gum arable carboxymethyl cellulose (CMC), ge la gum,
pectin, carrageenan, ghatti gum, guar gum, xanthan gum, locust gum, agar, starch,
alginate, cellulose, modified starch, or the combination thereof.
[ )5 5] Clause 9 ; The method of clause 8 wherein the stabilizer is gum Arabic.
[056] Clause 0 : The method of clause 8 wherein the stabilizer is CMC wherein CMC is
present in the micro-dispersion is in the range of 0 1-3% w/w and the viscosity of the
dispersion is in the range of 10-1000 cPs
[057] Clause 11; The method of any of clauses 1- 0 wherein the sorbate or benzoate
solution is combined with the stabilizer solution under high shear mixing at p 2.5-
4.0.
[058] Clause 12; The method of any of clauses 1-1 further comprising homogenizing the
sorbic acid or benzoic acid dispersion at 3000-10000 psi to reduce the particle size in
the dispersion to 0.1 to 50 microns.
[059] Clause 13: The method of any of clauses 1-12 wherein th micro-dispersion further
comprises a preservative selected from the group consisting of sodium
hexametaphosphate, calcium/sodium (Ca/Na EDTA), and lauroyl arginine ethyl ester
(LAE).
[060] Clause 14; The method of any of clauses 1- comprising in a . solubilizing a sorbate
and a benzoate in water.
[06 ] Clause 15: The method of any of clauses - 14 wherein the micro-dispersion is stable
for at least 40 days at days at 35 to 0 °F with no settling precipitates, or phase
separation.
[062 Clause 6 : A method of making beverage syrup comprising preparing a sorbic acid
dispersion in accordance with the method of clause 1 and adding the sorbic acid
dispersion to a syrup to provide a concentration of 0.10-0.5 t% (1000-5000 ppm)
sorbic acid based on total weight of the beverage syrup.
[063] Clause A beverage syrup prepared in accordance with the method of clause 6
wherein the syrup is stable for at least 40 days at days at 35 to 0 °F with no
creaming precipitates, or phase separation.
[064] Clause 18: A method of making a soft drink beverage comprising adding 3-7 parts
carbonated water or treated water to 1 part of the beverage syrup formed in clause
16.
[065] Clause 19: The method of clause 18 wherein the beverage contains 0.005-0.08 wt%
(50-800 ppm) sorbic acid based on total weight of the beverage.
[066] Clause 20: A method of making a beverage non-nutriti ve syrup comprising preparing
a sorbic acid dispersion in accordance with the method of clause 1 and adding the
sorbic acid dispersion to a non-nutritive syrup to provide a concentration of 0 0 5
wt% (1000-5000 pp ) sorbic acid based on total weight of the beverage syrup.
[067] Clause 2 ; A method of making a soft drink beverage comprising adding 20-60 parts
carbonated water or treated water to 1 part of the non-nutritive beverage syrup
formed in clause 20.
[068] Clause 22: A method of making beverage syrup comprising preparing a benzoic acid
dispersion in accordance with the method of clause 1 and adding the benzoic acid
dispersion to a syrup to provide a concentration of 0.1-0.5 wt% ( 000-5000 ppm)
benzoic acid based on total weight of the beverage syrup.
069] Clause 23: A beverage syrup prepared in accordance with the method of clause 22
wherein the syrup is stable for at least 40 days at days at 35 to 0 °F with no
creaming, precipitates, or phase separation
[070] Clause 24: A method of making a soft drink beverage comprising adding 3-7 parts
carbonated water or treated water to 1 part of the beverage syrup formed in clause
2
[071] Clause 25: The method of clause 2 1 wherein the beverage contains 0.005-0.08 wt%
(50-800 ppm) benzoic acid based on total weight of the beverage.
[072] Clause 26: A method of making beverage non-nutritive syrup comprising preparing a
benzoic acid dispersion in accordance with the method of clause 1 and adding the
benzoic acid dispersion to a non-nutritive syrup to provide a concentration of 0 1-0.5
wt% (1000-5000 ppm) benzoic acid based on total weight of the beverage syrup.
[073] Clause 27: A method of making a carbonated soft dri k beverage comprising adding
20-60 parts carbonated water to part of the non-nutritive beverage syrup formed in
clause 26,
[074] Clause 28: A stable beverage syrup comprising 1000-5000 ppm sorbic acid wherein
the syrup is stable for at least 40 days at days at 35 to 10 °F with no creaming,
precipitates, or phase separation
[075] Clause 29: A stable beverage comprising 200-800 pprn sorbic acid wherein the
beverage is stable for at least 40 days at days at 35 to 0 °F with no creaming,
precipitates, or phase separation.
[076] Example 1
[077] 8.3% Sorbic Acid/9.3% Gum Arabic Dispersion
[078] In a 200 mi beaker, 30 g potassium sorbate and 25 g water were added. Sorbate
mixture was heated (45-60 °C) until completely dissolved. Sorbate solution was
slowly added into 100 g gum arabic solution (25%) and 50 g citric acid solution
(30%) under high shear mixing. The dispersion pH was kept between 3-4 by adding
citric acid and temperature maintained below 60 °C. After completing addition of
potassium sorbate solution, the dispersion slurry was further mixed for 3-5 minutes.
The final sorbic acid dispersion pH was adjusted 2.8-3.5.
[079 Example 2
[080] 0. 5% Sorbic Acid Syrup
[081 In a 1000 mL beaker, 312 g sucrose, 1.3 g potassium citrate, 4.3 g citric acid, l g
Example 1 sorbic acid dispersion, and 289 g water. The mixture was mixed at room
temperature until all ingredients dissolved.
[082] Example 3
[083] Carbonated Soft Drink with 250 ppm Sorbic Acid
[084] Concentrated syrup (150 mL Example 2) was diluted into 750 m carbonated water
resulting in finished beverage.
[085] Example 4
[086] 8 1% Sorbic Acid/4 5% Gum Arabic Dispersion
[087] In a 200 ml beaker, 30 g potassium sorbate and 30 g water were added Sorbate
mixture was heated (45-60 °C) until completely dissolved. Sorbate solution was
slowly added into 50 g gum arable solution (25%) and 100 g citric acid solution
(30%) under high shear mixing. The dispersion pH was kept between 3-4 by adding
citric acid and temperature maintained below 60 °C. After completing addition of
potassium sorbate solution, the dispersion slurry was further mixed for 3-5 minutes.
The final sorbic acid dispersion pH was adjusted 2.8-3.5.
[088] Example 5
[089] 10.5% Sorbic Acid/5.8% Gum Arabic Dispersion
[090] In a 200 ml beaker, 30 g potassium sorbate and 30 g water were added. Sorbate
mixture was heated (45-60 C) until completely dissolved. Sorbate solution was
slowly added into 50 g gum arable solution (25%) and 50 g citric acid solution (30%)
under high shear mixing. The dispersion pH was kept between 3-4 by adding citric
acid and temperature maintained below 60 °C. After completing addition of
potassium sorbate solution, the dispersion slurry was further mixed for 3-5 minutes.
The final sorbic acid dispersion pH was adjusted 2.8-3.5.
[091] Example 6
[092] .8% Sorbic Acid/3 .8% Gum Arabic Dispersion
[093] In a 500 ml beaker, 90 g potassium sorbate and 170 g water were added. Sorbate
mixture was heated (45-60 °C) until completely dissolved. Sorbate solution was
slowly added into 150 g gum arable solution (25%) and 150 g citric acid solution
(30%) under high shear mixing. The dispersion pH was kept between 3-4 by adding
citric acid and temperature maintained below 60 °C. After completing addition of
potassium sorbate solution, the dispersion slurry was further mixed for 3-5 minutes
and then homogenized at 3000-5000 psi. The final sorbic acid dispersion p was
adjusted 2.8-3.5.
[094] Example
[095] 6.8% Sorbic Acid/5.5% Gu Arabic Dispersion
[096] n a 500 mi beaker, 90 g potassium sorbate and 170 g water were added. Sorbate
mixture was heated (45-60 °C) until completely dissolved. Sorbate solution was
slowly added into 220 g g m arable solution (25%) and 200 g citric acid solution
(30%) under high shear mixing. The dispersion pH was kept between 3-4 by adding
citric acid and temperature maintained below 60 °C. After completing addition of
potassium sorbate solution, the dispersion slurry was further mixed for 3-5 minutes
and then homogenized at 3000-5000 psi. The fmal sorbic acid dispersion pH was
adjusted 2.8-3.5.
[097] Example
[098] 6.8% Sorbic Acid/7.5% Gum Arabic Dispersion
[099] In a 500 ml beaker, 90 g potassium sorbate and 11 g water were added. Sorbate
mixture was heated (45-60 °C) until completely dissolved. Sorbate solution was
slowly added into 300 g gum arable soiution (25%) and 150 g citric acid soiution
(30%) under high shear mixing. The dispersion pH was kept between 3-4 by adding
citric acid and temperature maintained belo 60 °C. After completing addition of
potassium sorbate solution, the dispersion slurry was further mixed for 3-5 minutes
and then homogenized at 3000-5000 psi. The final sorbic acid dispersion pH was
adjusted 2.8-3.5.
[0100] Example 9
[0101] 9.6% Sorbic Acid/5.3% Gum Arabic Dispersion
[0102] In a 500 ml beaker, 90 g potassium sorbate and 0 g water were added. Sorbate
mixture was heated (45-60 °C) until completely dissolved. Sorbate solution was
slowly added into 150 g gum arable solution (25%) and 150 g citric acid solution
(30%) under high shear mixing. The dispersion pH was kept between 3-4 by adding
citric acid and temperature maintained below 60 °C. After completing addition of
potassium sorbate solution, the dispersion slurry was further mixed for 3-5 minutes
and then homogenized a 3000-5000 psi. The final sorbie acid dispersion pH was
adjusted 2.8-3.5
[0103] Example 10
[0104] 4.7% Sorbic Acid/9.3%! Gum Arabic Dispersion
[0105] n a 200 m beaker, 34 g potassium sorbate and 56 g water were added. Sorbate
mixture was heated (45-60 °C) until completely dissolved. Sorbate solution was
slowly added into 200 g gum arable solution (25%) and 200 g citric acid solution
(30%) under high shear mixing. The dispersion pH was kept between 3-4 by adding
citric acid and temperature maintained below 60 °C. After completing addition of
potassium sorbate solution, the dispersion slurry was further mixed for 3-5 minutes.
The final sorbic acid dispersion pH was adjusted 2.80.
[0106] Example
[0107] 5.7% Sorbie Acid/ 2 8% Gum Arabic Dispersion
[0108] In a 200 ml beaker, 30 g potassium sorbate and 60 g water were added. Sorbate
mixture was heated (45-60 °C) until completely dissolved. Sorbate solution was
slowly added into 200 g gum arable solution (25%) and 60 g citric acid solution
(50%) under high shear mixing. The dispersion pH was kept between 3-4 by adding
citric acid and temperature maintained below 60 °C, After completing addition of
potassium sorbate solution, the dispersion slurry was further mixed for 3-5 minutes
and then homogenized at 3000 psi. The final sorbic acid dispersion pH was adjusted
3.05.
[0109] Example 12
[0110] 7.8% Sorbic Acid/11.8% Gum Arabic Dispersion
[0111 In a 200 ml beaker, 44 g potassium sorbate and 46 g water were added. Sorbate
mixture was heated (45-60 °C) until completely dissolved. Sorbate solution was
slowly added into 200 g gum arabic solution (25%) and 60 g citric acid solution
(50%) under high shear mixing. The dispersion pH was kept between 3-4 by adding
citric acid and temperature maintained below 60 °C. After completing addition of
potassium sorbate solution, the dispersion slurry was further mixed for 3-5 minutes
and then homogenized at 3000 psi. The final sorbic acid dispersion p was adjusted
3.00.
0112] Example 13
[01131 7.4% Benzoic Acid/12.2% Gum Arabic Dispersion
[0114] n a 200 ml beaker, 36 g sodium benzoate and 63 g water were added. Sodium
benzoate mixture was heated (45-60 °C) until completely dissolved. Benzoate
solution was slowly added into 200 g gum arabic solution (25%) and 60 g citric acid
solution (50% under high shear mixing. The dispersion pH was kept between 3-4 by
adding citric acid and temperature maintained below 60 °C. Alter completing
addition of sodium benzoate solution the dispersion slurry was further mixed for 3-5
minutes and then homogenized at 3000 psi. The final benzoic acid dispersion pH was
adjusted to 3.00.
[0115] Example 14
[0116] 0.165% Sodium Benzoate Non-nutritive Syrup
[0117] In a 1000 mL beaker, 5.4 g aspartame, 1.4 g acesuifame potassium, 9.4 g Example 13
benzoic acid dispersion, and 483.8 g water. The mixture was mixed at room
temperature until all ingredients dissolved. The solution pH was adjusted 3.85 by
phosphoric acid (50%).
[0118] Example 5
[0119] 0.165% Potassium Sorbate Non-nutritive Syrup
[0120] n a 1000 beaker 5.4 g aspartame, 1.4 g acesuifame potassium. 7.9 g Example 12
sorbic acid dispersion, and 485.3 g water. The mixture was mixed at room
temperature until all ingredients dissolved. The solution pH was adjusted 3.85 by
phosphoric acid (50%).
[0121] Example 6
[0122] 10.7% Benzoic Acid/17.5% Gum Arabic Dispersion
[0123] In a 200 ml beaker, 30 g sodium benzoate and 74 g water were added. Sodium
benzoate mixture was heated (45-70 °C) until completely dissolved. Benzoate
solution was slowly added into 40 g gu arable solution (35%) and 25 g phosphoric
acid solution (50%) under high shear mixing. The dispersion pH was kept between 3-
4 by adding phosphoric acid and temperature maintained below 60 °C. After
completing addition of sodium benzoate solution, the dispersion slurry was further
mixed for 3-5 minutes. The final benzoic acid dispersion pH was adjusted to 3.00.
[0124] Example 17
[0125] 0.165% Sodium Benzoate Non-nutritive Syrup
[0126] in a 1000 mL beaker, 5.4 g aspartame, 0.55 g antifoam (Momentive SAG 710), and
485 g water were added. The mixture was heated at 32-40 °C until aspartame
dissolved. Then, 1.4 g acesuifame potassium, 7.69 g Example 16 benzoic acid
dispersion were added. The mixture was mixed for 30 minutes at 25-35 C The
solution pH was adjusted 3.9 by sodium hydroxide (3N). The non-nutritive syrup
was diluted with carbonated water in a 1:30 throw resulting in CSD beverage.
[0127] Example 18
[0128] 0 165% Sodium Benzoate Non-nutritive Syrup
[0129 In a 1000 n L beaker, 4.88 g aspartame, 0.725 antifoam (Momentive SAG 710),
and 459 g water were added. The mixture was heated at 32-40 °C until aspartame
dissolved. Then, 1.4 g acesulfame potassium, 26 06 g s cra ose (25%), and 7.69 g
Example 16 benzoic acid dispersion were added. The mixture was mixed for 30
minutes at 25-35 °C. The solution pH was adjusted 3 9 by sodium hydroxide (3N).
The non-nutritive syrup was diluted with carbonated water in a :40 throw resulting
in CSD beverage.
[0130] Example
[0131] 8.1% Sorbic Acid/12.3% Gum Arabic Dispersion
[0132] In a 200 ml beaker, 44 g potassium sorbate and 46 g water were added. Sorbate
mixture was heated (45-60 Cj until completely dissolved. Sorbate solution was
slowly added into 200 g gum arabic solution (25%) and 30 g phosphoric acid
solution (50%) under high shear mixing. The dispersion pH was kept between 3-4 by
adding phosphoric acid (50%) and temperature maintained below 60 °C. After
completing addition of sorbate solution, the dispersion slurry was further mixed for
3-5 minutes and then homogenized at 3000 psi. The final sorbic acid dispersion pH
was adjusted 3.00.
[0133] Example 20
[0134] 10% Sorbic Acid/1. 35% CMC Dispersion
[0135] In a 200 ml beaker, 44 g potassium sorbate and 46 g water were added. Sorbate
mixture was heated (45-60 °C) until completely dissolved. Sorbate solution was
slowly added into 200 g pre-hydrated carboxy methyl cellulose (Cekol 2000) solution
(2.22% CMC) an 30 g phosphoric a id solution (50%) under high shear mixing.
The dispersion pH was kept between 3-3.5 by adding phosphoric acid (50%) and
temperature maintained below 60 °C. The fi na sorbic aci dispersion pH was
adjusted 3.00.
[0136] Example 2 1
[0137] 8.2% Benzoic acid/0.74% CMC Dispersion
[0138] In a 200 ml beaker, 33 g sodium benzoate and 80 g water were added. Benzoate
mixture was mixed at room temperature until completely dissolved. Benzoate
solution was slowly added into 193 g pre-hydrated carboxymethyl cellulose (Cekol
2000) solution ( 1.3% CMC) and 30 g phosphoric acid solution (50%) under high
shear mixing. The dispersion pH was kept between 3-3.5 by adding phosphoric acid
(50%) and temperature maintained below 60 °C. The final benzoic acid dispersion
pH was adjusted 3.00.
[0139] Example 22
[0140] 8.3% Benzoic acid/0.69% CMC Dispersion
I a 200 ml beaker, 36 g sodium benzoate and 80 g water were added. Benzoate mixture was
mixed at room temperature until completely dissolved. Benzoate solution was slowly added
into 203 g pre-hydrated carboxymethyl cellulose (Cekoi 2000) solution (1.09% CMC) and
30 g phosphoric acid soiution (50%) under high shear mixing The dispersion pH was kept
between 3-3.5 by adding phosphoric acid (50%) and temperature maintained below 60 °C.
The final benzoic acid dispersion pH was adjusted 3.00.
[0141] Example 23
[0142] 8.4% Benzoic acid/0.59% CMC Dispersion
[0143] In a 200 m beaker, 36 sodium benzoate and 80 g water were added. Benzoate
mixture was mixed at room temperature until completely dissolved. Benzoate
solution was slowly added into 202 g pre-hydrated carboxymethyl cellulose (Cekol
2000) soiution ( 1.04% CMC) and 30 g phosphoric acid solution (50%) under high
shear mixing. The dispersion p was kept between 3-3.5 by adding phosphoric acid
(50%) and temperature maintained below 60 °C. The final benzoic acid dispersion
pH was adjusted 3.00.
[0144] Example 24
{0145] 7.8% Benzoic acid/0.93% CMC Dispersion
[0146] In a 200 ml beaker, 30 g sodium benzoate and 80 g water were added. Benzoate
mixture was mixed at room temperature until completely dissolved. Benzoate
solution was slowly added into 200 g pre-hydrated carboxymethyl cellulose (Cekol
2000) solution (1.5% CMC) and 30 g phosphoric acid solution (50%) under high
shear mixing. The dispersion pH was kept between 3-3.5 by adding phosphoric acid
(50%) and temperature maintained below 60 °C. After completing addition of
benzoate solution, the dispersion slurry was further mixed for 3-5 minutes and then
homogenized at 3000 psi. The final benzoic acid dispersion pH was adjusted 3.00.
[0147] Example 25
[0148] 0.15% Sorbic Acid/0.3% Sodium Hexametaphosphate/0.01 8% Ca/Na EDTA Syrup
[0149] In a 1000 mL beaker, 312 g sucrose, 1 3 g potassium citrate, 4.3 g citric acid, 9 6 g
Example 9 sorbic acid dispersion, 1.8525 g sodium hexametaphosphate, 0.1 12 g
Ca/Na EDTA, and 288 g water. The mixture was mixed at room temperature until
all ingredients dissolved.
[0150] Example 26
[0151] Carbonated Soft Drink with 250 ppm Sorbic Acid/500 pp Sodium
Hexametaphosphate/30 ppm Ca/Na EDTA
[0152] Concentrated syrup (150 mL Example 10) was diluted into 750 mL carbonated water
resulting in finished beverage.
[0153] Example 2
[0154] This example demonstrates the solubility and stability of sorbic acid powder and
sorbic acid dispersions prepared from potassium sorbate in water one sample,
sorbic acid powder was added directly to water. In a second sample, sorbic acid was
formed from solubilizing potassium sorbate and converting the sorbate to sorbic acid
without a stabilizer In a third sample, sorbic acid was formed from solubilizing
potassium sorbate and converting the sorbate to sorbic acid with a stabilizer. As can
be seen in th table below, sorbic acid dispersion with gum arabic provided a stable
solution having a viscosity of less than 50 p
[0155] Example 28
[0156] This example demonstrates the stability of sorbic acid dispersions in finished
beverages. Sorbic acid dispersions were tested in finished beverages at temperatures
of 40 70. and 90 F at concentrations of 200-560 pprn. There were no precipitates
over the storage time of 40 days. Beverages containing the sorbic acid dispersions
and caffeine were also stable and clear.
7 1
[0157] Example 29
[0158] This example demonstrates the compatibility of a sorbic acid dispersion combined
with other preservatives sodium hexametaphosphate (SHMP) and calcium/sodium
EDTA (Ca/Na EDTA) in preservative cocktail system. Both the concentrated syrup
and finished beverage prepared with the sorbic acid dispersion and sodium
hexametaphosphate (SHMP) and Ca Na EDTA were shelf stable with no precipitates
over time.
[0159] Example 30
[0160] The viscosity of a sorbic acid dispersion having 6.7 wt% solids was tested over
various temperatures. The results show that the sorbic acid dispersion has a low
viscosity which increases slightly with decreasing temperature. As shown in Fig 1,
the sorbic acid dispersion had less than 20 cPs viscosity between temperatures of 40-
90 °F.
[0161] Example 3
[0162] The viscosity of sorbic acid dispersions having at 6.7% solids and different amounts
of gum arable were tested at 23 °C. The dispersion viscosity slightly increases with
increasing gum arabic. Fig. 2 demonstrates that the sorbic acid dispersion exhibited
low viscosity with gum arabic in the range of 3.75-7.50 w/w%.
Sorbic Acid/Benzoic Acid Dispersion Stability (Aged 20 days at 25 °C)
While the invention has been described with respect to specific examples including
presently preferred modes of carrying out the invention, those skilled in the art will
appreciate that there are numerous variations and permutations of the above
described systems and techniques that fall within the spirit and scope of the invention
as set forth in the appended claims.

claims:
A method of preparing a stabi lized micro-dispersion comprising
a . solubilizing a sorbate or benzoate in water to form a sorbate or benzoate
solution, wherein the temperature of the water is 20 to 00 °C;
b. combining a stabilizer with water to form a stabilizer solution, wherein the
stabilizer is a biopolymer or a modified polysaccharide;
c. combining the sorbate or benzoate solution and stabilizer solution and
mixing to form a sorbic acid or benzoic acid micro-dispersion comprising
0.1 to 25 wt% stabilizer and 1 to 30 t% sorbic acid or benzoic acid, each
base on total weight of the micro-di spersion; and
d. adjusting the pH of the micro-dispersion to 2.5 to 4, wherein the viscosity
of the dispersion is no greater than 1000 cPs at 25 °C.
The method of claim 1 wherein the viscosity of the micro-dispersion is no greater
than 100 cPs at 5 °C.
The method of claim 1 or clai 2 wherein the micro-dispersion comprises 1 to 30
wt stabilizer based on total weight of the micro-dispersion.
The method of any of claims 1-3 wherein the micro-dispersion comprises 5 to 15
wt sorbic acid or benzoic acid, each based on total weight of the microdispersion.
The method of any of claims 1-4 comprising in a . solubilizing potassium sorbate
to form a solution comprising 30-65 wt% potassium sorbate or a . solubilizing
sodium or potassium benzoate to form a sodium or potassium benzoate solution to
form a benzoate solution comprising 30-65 wt% sodium or potassium benzoate.
The method of any of claims 1-5 wherein, in step a, the temperature of the water
is 20 to 70 °C
7. The method of any of claims 1-6 wherein the stabilizer is selected from the group
consisting of gum arable, carboxymethyi cellulose (CMC), gellan gum, pectin
carrageenan, ghatti gum, guar gum, xanthan gum locust gum, agar, starch
alginate, cellulose, modified starch, or the combination thereof.
8. The method of claim 8 wherein the stabilizer is gum Arabic or CMC wherein
CMC is present in the micro-dispersion is in the range of 0.1-3% w/w and the
viscosity of the dispersion is in the range of 10-1000 cPs.
9. The method of any of claims 1-8 wherein the sorbate or benzoate solution is
combined with the stabilizer solution under high shear mixing at pH 2.5-4.0
0. The method of any of claims 1-9 further comprising homogenizing the sorbic acid
or benzoic acid dispersion at 3000-10000 psi to reduce the particle size in the
dispersion to 0.1 to 50 microns.
11. The method of any of claims 1-10 wherein the micro-dispersion further comprises
a preservative selected from the group consisting of sodium hexametaphosphate,
calcium/sodium (Ca a EDTA), and lauroyl arginine ethy ester (LAE).
12. The method of any of claims 1-1 wherein the micro-dispersion is stable for at
least 40 days at days at 35 to 110 °F with no settling, precipitates, or phase
separation.
13. A method of making beverage syrup comprising preparing a sorbic acid
dispersion in accordance with the method of claim 1 and adding the sorbic acid
dispersion to a syrup to provide a concentration of 0.10-0 5 wt% (1000-5000 ppm)
sorbic acid based on total weight of the beverage syrup; or preparing a benzoic
acid dispersion in accordance with the method of claim 1 and adding the benzoic
acid dispersion to a syrup to provide a concentration of 0.1-0.5 wt% (1000-5000
ppm) benzoic acid based on total weight of the beverage syrup.
14. A method of making a soil drink beverage comprising adding 3-7 parts carbonated
water or treated water to 1 part of the beverage syrup formed in claim ; or
adding 20-60 parts carbonated water or treated water to 1 part of the beverage
syrup formed in claim 13 , wherein the syrup is a non-nutritive syrup.
5. The method of claim 14 wherein the beverage contains 0.005-0.08 wt% (50-800
ppm) sorbic acid or benzoic acid based on total weight of the beverage.
16. A stable beverage syrup comprising 1000-5000 ppm sorbic acid or 200-800 ppm
sorbic acid wherein the syrup is stable for at least 40 days at days at 35 to 10 °F
with no creaming, precipitates, or phase separation.