GB2103917A - Aspartame concentrates for carbonated beverages - Google Patents

Abstract

Bottling and fountain syrups for making aspartame-sweetened carbonated beverages are prepared by first preparing an aspartame concentrate, containing from about one part by weight to about three parts by weight of aspartame and about ten parts by weight of a carbonated beverage acidulent solution having a pH of from about 1.5 to about 2.2; diluting the aspartame concentrate with water, and adding flavoring and coloring agents to produce a bottling or fountain syrup. Also disclosed are aspartame concentrate solutions and bottling syrups and beverages produced therefrom.

Description

SPECIFICATION Aspartame-sweetened carbonated beverages The present invention relates to aspartamesweetened carbonated beverages. More particularly, the invention relates to methods for preparing aspartame-sweetened carbonated beverage bottling or fountain syrups, and the concentrates used in such methods.

There is a growing preference by diabetic and diet-conscious consumers for a wide variety of food products sweetened with low calorie sweeteners instead of sucrose or other sugars.

This trend has been especially prevalent with respect to non-alcoholic sweetened carbonated beverages. The present invention concerns carbonated beverages sweetened with dipeptide sweeteners, such as those generally described in United States Patent No. 3,475,403. Such dipeptide sweeteners include the lower alkyl esters of aspartylphenylalanine. The methyl ester of this dipeptide (I-methyl-N-aspartyl-Lphenylalanine) is the most common form of the sweetener, and is generally referred to herein by its common name, aspartame. As used herein, the term aspartame is intended to include the lower alkyl esters of the dipeptide, as well as edible soluble salts thereof.

The sweetness of aspartame has been reported to be about 1 80 times that of sucrose, and consequently it has a very low caloric content on an equivalent sweetness basis. Accordingly, this material has been considered as an attractive substitute for sucrose and other sugars in a wide variety of food products and beverages.

Aspartame suffers from two primary disadvantages as a low calorie sweetener for food products. The dipeptide ester is subject to degradation in aqueous systems, particularly at low pH or high temperatures. Secondly, the compound has a very slow rate of dissolution in water. These disadvantages are particularly pronounced in carbonated beverage formulations, because of the high water concentrations and low pH's associated with such beverages.

The solubility of aspartame in water has been found to be dependent upon pH and temperature.

It has previously been reported that the solubility of aspartame in water is lowest at its isoelectric point at pH 5.2, and increase as pH is lowered with a maximum solubility at pH 2.2. Previous reports indicate that the solubility decreases as the pH is lowered further below 2.2. E.g., see product brochure for Equa 200 brand of aspartame, published by G. D. Searle 8 Co., Skokie, Illinois 60076. The solubility of aspartame is reported to increase as temperature is increased.

Previous method to stabilize and solubilize aspartame have generally involved mixing the sweetener with various food grade bulking agents.

For example, Glicksman, et al., U.S. Patent 3,761,288 describe a composition prepared by co-drying an aqueous solution of an edible bulking agent such as citric acid, dextrin, and various sugars, with aspartame. Furda, et al., U.S. Patent 3,934,048 describe a sweetening composition prepared by co-drying a solution of the sweetening compound with an edible, bland polysaccharide. When such compositions are employed in carbonated beverage formulations, the bulking agents may impart their own characteristic flavors to the product, which are foreign to the original product formulation and therefore may not be acceptable to the consumer.

Carbonated beverages are typically prepared by first making a so-called bottling or fountain syrup.

Such a syrup is an aqueous solution of a sweetening agent, an acidifying agent, flavoring concentrates, and optional colorings and preservatives. These syrups are generally concentrated, such that they may be diluted with water in a proportion of from about one volume to about three volumes of syrup per ten volumes of water. Carbonation is added to the beverage either by carbonating the diluted syrup or by using carbonated water as the diluent for the syrup.

Bottling and fountain syrups typically have pH's in the range of about 1.8 to about 2.5. In this pH range, the solubility of aspartame is reported to be about 6%. The amount of aspartame to be dissolved in such a syrup may vary considerably, depending upon the type of beverage being prepared, the degree of sweetness desired, and the presence or absence of other sweetening compounds. Generally, an aspartame concentration of about 0.2-0.5 w/v is employed in the bottling or fountain syrup, when aspartame is the sole sweetening agent. Aspartame may sometimes be used in conjunction with other sweeteners, such as saccharins, cyclamates or sugars. In such combination products, the aspartame concentration in the bottling or fountain syrup may be as low as about 0.04% or lower.

Although it is known that the solubility of aspartame increases as pH is lowered, this knowledge did not suggest the method of the present invention, which involves preparing an aspartame concentrate in a concentrated solution of the conventional beverage acidulent. First of all, the total amount of acidulent utilized in a bottling or fountain syrup cannot be substantially increased, without deleteriously affecting the quality of the beverage. Accordingly, the only method by which the acidulent can be concentrated to form a solution having a low pH is to reduce the volume. Reducing the volume concommitantly increases the necessary concentration of the aspartame. As indicated above, the maximum solubility of aspartame has previously been reported to be about 6% w/v at a pH of 2.2.Based upon these reports, one would expect that concentrating the beverage acidulent to a pH of 2.2 could necessitate an aspartame concentration in excess of its reported solubility.

Moreover, one would also expect another limitation for such concentrates to be the reported poor stability of aspartame at such low pH's.

Nevertheless, it has surprisingly been discovered that aspartame pre-mixes having concentrations as high as about 27% w/v can be prepared in a concentrated beverage acidulent solution having a pH of from about 1.5 to about 2.2. The solubility of aspartame has actually been found to increase as pH is lowered below 2.2. This discovery has provided a means for preparing a bottling or fountain syrup, which invoives first preparing an aspartame concentrate in a concentrated, highly acidic solution of the beverage acidulent, followed by dilution of the aspartame concentrate with water and addition of flavorings and coloring agents to form the finished bottling or fountain syrup. Aspartame has been found to quickly dissolve in such concentrates, without the need for heating.An additional advantage of preparing such a concentrate, is that the lower volumes permit the use of high speed mixing or homogenizing equipment to create high shear rates, which further accelerate the dissolution of the aspartame.

The aspartame concentrates of the present invention are prepared by dissolving from about 0.25 part by weight to about 3 parts by weight of aspartame in about 10 parts by weight of a carbonated beverage acidulent solution. Lower aspartame concentrations may be used in conjunction with other sweetening agents. Higher aspartame concentrations are generally not achievable, because of solubility limitations.

Preferred aspartame concentrations range from about 1.0 part by weight to about 2.7 parts by weight of aspartame in about ten parts by weight of the carbonated beverage acidulent solution. The carbonated beverage acidulent solution is generally a concentrated solution of the conventional acidulent utilized in the particular beverage being prepared. This solution generally has a pH of from about 1.5 to about 2.2, which is conductive to a high solubility of aspartame. The preferred pH of the carbonated beverage acidulent solution ranges from about 1.7 to about 2.0. Any of the standard beverage acidulents may be employed, such as phosphoric acid, citric acid, malic acid, fumaric acid, or mixtures thereof.

Phosphoric acid is preferred, because the desired low pH's may be readily obtained using this acid.

As indicated above, it is not necessary to heat the solution to dissolve the aspartame, but heat may be applied if desired. For instance, a temperature from about 1 00C to about 500C may be employed. Relative long exposures to higher temperatures may adversely affect the stability of the aspartame. A preferred temperature range is from about 1 5 C to about 250C. Stirring the concentrate accelerates the dissolution rate of the aspartame, and high speed mixers or blenders may advantageously be employed.

To prepare a bottling or fountain syrup from the aspartame concentrate, generally from about 2 parts by volume to about 6 parts by volume of the aspartame concentrate is mixed with about 100 parts by volume of water. Flavoring concentrates may also be generally blended into this solution.

Such concentrates include materials such as concentrated cola flavoring, essential oils and extracts of various fruits and spices, as well as artificial flavors, such as ethyl acetate or amyl butyrate and concentrated fruit juices, all of which are well known in the art. Additionally, colors such as caramel coloring, or any of the various F.D. 8 C.

colors may be employed to obtain the desired coloring of the resulting beverage. If desired, preservatives, such as sodium benzoate, may also be added.

The methods and compositions of the present invention are further illustrated by the following examples which are not intended to be limited.

EXAMPLE I An aspartame-sweetened, carbonated, cola beverage was prePared as follows: Preparation of Aspartame Concentrate 1. Beverage quality water (10.0 Imperial gallons, 45.5 liters) having a temperature of at least 1 00C (500 F) was added to a 20 Imperial gallon stainless steel container; 2. Beverage quality phosphoric acid (80% w/v) (0.83 Imperial gallon, 3.8 liters) was added to the water with stirring. The acid container was rinsed with 0.83 Imperial gallon (3.8 liters) of water, which was added to the acid solution. The resulting solution had a pH between 2.1 and 2.2: 3. Aspartame (10.125 pounds, 4.597 kg) was slowly added to the acid solution with agitation.

All of the aspartame dissolved within thirty minutes or less.

Preparation of Bottling Syrup 1. Beverage quality water (353.0 Imperial gallons, 1 604.7 liters) was measured into a stainless steel mixing tank; 2. The aspartame concentrate was mixed with the water in the mixing tank, and the aspartame concentrate container was rinsed with 4.0 Imperial gallons (18.2 liters) of water, which was added to the mixing tank; 3. Cola concentrate (containing flavorings and caramel coloring) (3,331 Imperial gallons, 15.1 liters) was mixed with solution in the mixing tank.

The cola concentrate container was rinsed with 2.0 Imperial gallons (9.1 liters) of water, which was added to the mixing tank. This solution was slowly agitated for ten minutes to provide an aspartame-sweetened cola bottling syrup.

Bottling Operation 1. The above bottling syrup was diluted with water at a ratio of one part by volume syrup to five parts by volume water on a conventional bottling line, and filled into bottles and cans; 2. Sufficient carbon dioxide gas was added to provide a beverage containing 3.3 + 0.1 volumes of CO2.

EXAMPLE II The procedures of Example I for making an aspartame concentrate and bottling syrup were repeated in all essential details, except that the aspartame concentrate was prepared by adding 0.5 U.S. gallons (1.9 liters) of 80% phosphoric acid to 10 U.S. gallons (37.9 liters) of water, and dissolving 11.25 pounds (5.11 kg) of aspartame therein, while mixing in a high speed homogenizer mixer. All of the aspartame dissolved within thirty minutes or less after its addition.

EXAMPLE Ill The procedures of Example I for preparing an aspartame concentrate and a bottling syrup were repeated in all essential details, except that the aspartame concentrate was prepared by adding 0.5 U.S. gallons (1.9 liters) of 80% phosphoric acid to 7.5 U.S. gallons (28.4 liters) of water, and dissolving 11.25 pounds (5.11 kg) of aspartame therein, while mixing in a high speed homogenizer mixer. All of the aspartame dissolved within thirty minutes of its addition. Additional water was added to the mixing tank to make up for the reduced aspartame concentrate volume.

EXAMPLE IV The procedures of Example i for preparing an aspartame concentrate and a bottling syrup were repeated in all essential details, except that the aspartame concentrate was prepared by adding 0.5 U.S. gallons (1.9 liters) of phosphoric acid to 5.0 U.S. gallons (18.9 liters) or water, and dissolving 11.25 pounds (5.11 kg) of aspartame therein, while mixing in a high speed homogenizer mixer. All of the aspartame dissolved within thirty minutes of its addition. Additional water was added to the mixing tank to make up for the reduced aspartame concentrate volume.

EXAMPLE V The procedures of Example I for preparing an aspartame concentrate and a bottling syrup were repeated in all essential details, except that the aspartame concentrate was prepared by adding 1.0 U.S. gallons (3.79 liters) of phosphoric acid to 10 U.S. gallons (37.9 liters) of water, and dissolving 11.25 pounds (5.11 kg) of aspartame therein, while mixing in a high speed homogenizer mixer. All of the aspartame dissolved within thirty minutes of its addition. Additional water was added to the mixing tank to make up for the reduced aspartame concentrate volume. The resulting bottling syrup has a lower pH (2.6) than the bottling syrup of Example 1(3.0).

EXAMPLE VI The procedures of Example I for preparing an aspartame concentrate and a bottling syrup were repeated in all essential details, except that the aspartame concentrate was prepared by adding 1.0 U.S. gallons (3.79 liters) of phosphoric acid to 7.5 U.S. gallons (28.4 liters) of water, and dissolving 11.25 pounds (5.11 kg) of aspartame therein, while mixing in a high speed homogenizer mixer. All of the aspartame dissolved within thirty minutes of its addition. Additional water was added to the mixing tank to make up for the reduced aspartame concentrate volume. The resulting bottling syrup has a lower pH (2.6) than the bottling syrup of Example 1(3.0).

EXAMPLE VII The procedures of Example I for preparing an aspartame concentrate and a bottling syrup were repeated in all essential details, except that the aspartame concentrate was prepared by adding 1.0 U.S. gallons (3.79 liters) of phosphoric acid to 5.0 U.S. gallons (18.9 liters) of water, and dissolving 11.25 pounds (5.11 kg) of aspartame therein, while mixing in a high speed homogenizer mixer. All of the aspartame dissolved within thirty minutes of its addition. Additional water was added to the mixing tank to make up for the reduced aspartame concentrate volume. The resulting bottling syrup had a lower pH (2.6) than the bottling syrup of Example 1(3.0).

EXAMPLE VIII The procedures of Example I for preparing an aspartame-sweetened cola beverage are repeated in all essential details for the preparation of a citrus fruit flavored beverage, with the following exceptions: 10.0 pounds (4.54 kg) of citric acid is substituted for phosphoric acid, and 3.0 gallons of lemon/lime flavor concentrate is substituted for the cola concentrate. The procedure provided a pleasantly flavored carbonated citrus beverage.

Claims (14)

1. A method for making an aspartamesweetened carbonated beverage bottling or fountain syrup, comprising: (a) dissolving from about 0.25 part by wt. to about 3 parts by wt. of aspartame in about 10 parts by wt. of a carbonated beverage acidulent solution having a pH of from about 1.5 to about 2.2, to form an aspartame concentrate, and (b) mixing from about 2 parts by volume to about 6 parts by volume of the aspartame concentrate and a flavoring amount of a flavoring concentrate with about 100 parts by volume of water, to form an aspartamesweetened carbonated beverage bottling or fountain syrup.

2. The method of claim 1 , wherein the aspartame concentrate is prepared by dissolving from about 10. parts by wt. to about 2.7 parts by wt. of aspartame in about 10 parts by wt. of a carbonated beverage acidulent solution having a pH of from about 1.7 to about 2.0.

3. The method of claim 2, wherein the carbonated beverage acidulent solution is an aqueous solution of phosphoric acid, citric acid, malic acid, fumaric acid, or mixtures thereof.

4. The method of claim 2, wherein the aspartame is dissolved in the carbonated beverage acidulent solution at a temperature of from about 100Ctoabout500C.

5. The method of claim 4, wherein the aspartame is dissolved in the beverage acidulent at a temperature of from about 1 50C to about 25"C.

6. The method of claim 1, further comprising adding a saccharin or cyclamate sweetening agent or a sugar to the bottling or fountain syrups.

7. The method of claim 1, 2, or 5, further comprising in step (b), adding a coloring agent.

8. The method of claim 7, further comprising adding a preserving amount of a carbonated beverage bottling syrup or fountain syrup preservative to the aspartame concentrate or the bottling syrup or fountain syrup.

9. The method of claim 7, wherein the flavoring concentrate is a cola flavored concentrate, containing caramel color and the carbonated beverage aciduient solution is an aqueous phosphoric acid solution, thereby forming a cola bottling or fountain syrup.

10. A method for preparing an aspartamesweetened carbonated beverage, comprising (a) diluting from about 1 to about 3 parts by volume of a bottling or fountain syrup prepared by the method of claim 1, 2, 3, 4, 5 or 6 with about 10 parts by volume of water, to form an uncarbonated beverage, and (b) carbonating the uncarbonated beverage with about 2.5 to about 4.5 volumes of carbon dioxide gas.

11. A method for preparing an aspartamesweetened carbonated cola beverage, comprising: (a) diluting from about 1 to about 3 parts by volume of a bottling or fountain syrup prepared by the method of claim 9 with about 10 parts by volume of water, to form an uncarbonated cola beverage, and (b) carbonating the uncarbonated cola beverage with about 3 to about 4 volumes of carbon dioxide gas.

12. An aspartame concentrate comprising a solution of from about 0.25 part by wt. to about 3 parts by wt. of aspartame in about 10 parts by weight of a carbonated beverage acidulent solution, having a pH of from about 1.5 to about 2.2.

1 3. The aspartame concentrate of claim 12, wherein the aspartame solution contains from about 1.0 parts by wt. to about 2.7 parts by wt. of aspartame in about 10 parts by wt. of a carbonated beverage acidulent solution, having a pH of from about 1.7 to about 2.0.

14. The aspartame concentrate of claim 13, wherein the carbonated beverage acidulent solution is an aqueous solutions of phosphoric acid, citric acid, malic acid, fumaric acid, or mixtures thereof.

1 5. The aspartame concentrate of claim 12, further comprising a saccharin or cyclamate sweetening agent or a sugar.

1 6. An aspartame-sweetened carbonated beverage bottling or fountain syrup, prepared by the method of claim 1, 2, 3, 4, 5 or 6.

1 7. A method of making an aspartamesweetened, carbonated, beverage substantially as hereinbefore described.

1 8. An aspartame-sweetened, carbonated, beverage, bottling or fountain syrup when prepared by the method of the claims 1 to 11.