Method of purifying polydextrose and composition containing same.

BACKGROUND OF THE INVENTION

The present invention relates to the technique of preparing low calorie thickening agents for food products, and in particular to the preparation of a low calorie thickening agent which is organoleptically acceptable for use in sweetening compositions such as confectionery. .

In recent years, it has become increasingly important to people in almost every country in the ¹ _1 world be careful about food intake and food intake.

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The beverage industry has met requirements that stem from popular trends by making dietary non-alcoholic beverages that rely on high intensity sweeteners to replace sugar content. However, solid food manufacturers have not been so successful as sugar leads to thickening as well as sweetness which must be replaced by a low calorie thickening agent when sugar is removed.

To this end, an extremely low calorie thickening agent has been developed which is called polydextrose. Polydextrose is a sugar substitute and has many of the desirable technological properties of sugar but is not sweet. This unsweetened thickener capacity can be an advantage in; food products in which conventional compositions with!

Sugar based i are very sweet for some tastes. Thus in foods for which calories and sweetness are to be controlled, polydextrose * in combination with an artificial sweetener may preferably be used. Calories can often be reduced by 50% or more. '

Polydextrose is a non-nutritive carbohydrate substitute that can be prepared by polymerizing glucose in the presence of food grade polycarboxylic acid catalysts and polyols. See US Patent No. 3,766,165 and US Patent No. 3,876,794. Generally, polydextrose is known to exist in two forms, Polydextrose A, a solid, and Polydextrose N, a 70% solution, both of which also include low molecular weight components such as glucose, sorbitol and oligomers. !

Unfortunately, the ability to use polydextrose is hindered by its innate bitter taste.

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acceptable and sour aroma when used in a sufficient amount, which may be attributed to low molecular weight compounds, for example, less than 1,000 µm remaining after production. Bitter taste may be associated with endogenous levoglucosan (1,6-anhydroglycosis), while small amounts of furfural derivatives may be responsible for sour flavors.

U.S. Patent 4,622,233 to Torres discloses a first process for treating Type A polydextrose by bleaching with a bleaching agent and further purifying. Another process is presented and claimed in Torres Patent 233 for reducing the color, glucose content and anhydrous glucose content of Type A polydextrose including:

(a) contacting a 60-70% (w / w) aqueous solution of Type A polydextrose with a food grade bleach at a temperature of 25-90 ° C and a pH value of about from 2.5 to about 9.0;

(b) adjusting the pH of the product of step (a), if above 7, to about 6;

(c) adding one or more of the solvents chosen from the group consisting of methanol, ethanol and ethyl acetate such that these solvents include 50-80% (w / w) of the mixture; and (d) filter the final product, and, if desired, dry. Unfortunately, however, Torres Patent 233 links discoloration to purification, which is not necessary, and which may be an undesirable process requirement. For example, when polydextrose is heated to a high temperature, such as cooking, the color returns to the substance. In many cases, there is no need for discoloration. In addition, additional steps are required by the 3 -

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Tower processes that require additional time, handling, and energy.

It has now been found, however, that polydextrose can be purified in essentially one phase to remove unpleasant organoleptic characteristics ie to produce a purified product which is particularly useful in, among other things, confectionery products such as hard candy. . j

II SUMMARY OF THE INVENTION |

The present invention is a process for purifying polydextrose, and the resulting purified product to remove remaining contaminants from its production is sufficient to produce an organoleptically acceptable polydextrose ingredient. 0 The process of the present invention includes contacting an aqueous polydextrose solution at a concentration of from about 10% to about 90% with a polar organic solvent in a polydextrose to solvent ratio of from about 5 to 45% by weight of polydextrose to about about 35 to 85% by weight of the solvent. The mixture is then allowed to equilibrate to coat a fraction containing essentially contaminants and a fraction containing essentially polydextrose, followed by separation of the fractions for use from the polydextrose containing fraction.

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In preferred methods of the present process, ethanol and acetone may be used as polar solvents. When using ethanol, the concentration of aqueous polydextrose is preferably from about 12.5% ​​to about 83%, and the ratio of polydextrose to solvent is about 5 to 25 parts by weight of polydextrose to about 45 to about 85 parts by weight of the solvent.

More preferably when using ethanol, the concentration of polydextrose in water is about

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14% to about 50%, and the ratio of polydextrose to solvent is from about 5 to about 15 parts by weight of polydextrose to about 55 to about 75 parts by weight of solvent.

When acetone is used as a solvent, the concentration of polydextrose is preferably | about 10% to about 62.5%, and the ratio of polydextrose I to solvent is from about 5 to about 25 parts by weight!

of polydextrose to about 55 to about 75 parts by weight of the solvent. Most preferably the concentration of polydextrose in solution in water is from about 10% to about 57.5% and the ratio of polydextrose to solvent is from about 5 to about 65 parts by weight of polydextrose to about 45 to about 45%. 65 parts by weight of the solvent.

After contacting the aqueous polydextrose solution and solvent, for example by high speed mixing, may be allowed to equilibrate for a period of time from about 0.25 to about 48 hours at a temperature of from about -15 ° C to about 75 ° C, preferably such an equilibrium is conducted from about 0 ° C to about 50 ° C, and most preferably between about 20 ° C to about 50 ° C. 0 Equilibrium time is from about 10 to about 56 hours, and most preferably from about 12 to about 24 hours. Separation may be conducted for example by decanting an upper phase of the fraction containing essentially contaminants from the container.

In a preferred embodiment separation may be accelerated by centrifugation.

Removal of low molecular weight compounds that are contaminants produced during production makes purified polydextrose difficult to handle in certain cases after purification. It has been found that when using purified polydextrose for use in a hard candy, various compounds can be added later.

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low molecular weight grades to the purified form to facilitate their use in hard candy compositions. For example, low molecular weight compounds such as glycerine, polyhydric alcohols, monosaccharides, and disaccharides may be added in amounts of from about 1 to about 40% by weight of the final hard candy composition, preferably no more than 10%. 20 $ and most preferably no more than 10 $ of candy composition.

Although the purified polydextrose solution prepared according to the process of the invention may be used in any food product suitable for inclusion, it has been found that its use in confectionery products requiring an agent was especially effective in the present invention. sugar thickener which has been replaced by a high intensity sweetener. Thus, the polydextrose of the present invention may conveniently be used in a gum, tablet and candy product such as hard candy, chocolate and nougat as described above.

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When used in these products, intensive sweeteners including acesulfame-K, aspartame, saccharin, or other intense sweeteners may be used. Hard candy of the present invention may also contain acids such as citric acid, isocitric acid, maleic acid, fumaric acid, succinic acid, adipic acid, malic acid, and tartaric acid, with citric acid being the preferred acid for use in a hard candy. along with purified polydextrose. Other ingredients that may be used in the present composition include flavorings, colorings and salt which are known for use in confectionery compositions.

As a result of the present invention food products containing 50% or more of polydextrose can be obtained as organoleptically acceptable by removing the bitter taste and sour wire inherent in polydextrose.

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are contaminants that remain in the production process, in- eluting endogenous levoglucosan (1,6-anhydroglucose), and small amounts of furfural derivatives that appear to be responsible for the sour aroma.

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Furthermore, the process of the present invention is presented in such a way as to remove the need for bleaching of the polydextrose ingredient by bleaching and the appropriate process steps which require the production of undesirable salt constituents. Moreover, the present process can be achieved very simply without the need for a filtration phase.

In addition, as a result of the present invention, a hard candy is presented which is truly a low calorie hard candy. In addition, the hard candy product of the present invention can be processed very efficiently without unnecessary additional steps of filtration and / or use of pH control agents which may introduce undesirable salts into the candy composition.

For a better understanding of the present invention, along with other additional objects, reference is made to the following description taken in conjunction with the accompanying drawings, and its scope will be set forth in the appended claims.

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I BRIEF DESCRIPTION OF DRAWINGS

Figure 1A is a ternary phase diagram showing achieved phase separation for experimental batches according to the present invention using ethanol as a solvent;

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Α Figure lb is a ternary diagram of | stages presenting the organoleptically acceptable batches successfully obtained for the experiments presented in

Figure 1a

Figure 2a is a ternary phase diagram showing separation of phases for experimental batches according to the present invention using acetone as solvent; and !

Figure 2b is a ternary 1-phase diagram showing the organoleptically successful lots obtained from the experiments shown in Figure 2a.

DETAILED DESCRIPTION OF THE INVENTION

In the first aspect, the present invention is a process for purifying polydextrose to a form that is highly used in the preparation of food products for which the use of a thickening agent is suitable. The procedure is improved by the fact that it is a simple operation which includes treating a polydextrose solution with polar organic solvents such as alcohols and ketones and which is effective in removing the aroma of commercially produced polydextrose.

A general procedure according to the present invention includes dissolving the polydextrose in deionized water (pH 2.5-3.0, unadjusted) and mixing the resulting solution with a polar organic solvent in a specific ratio. The mixture may be vigorously stirred until a homogenized emulsion is formed and then set aside to equilibrate. A suitable time interval for maximum product recovery is required which may vary in its broadest aspect from 0.25 to 48 hours, and in a more preferred range from 10 to 36 hours, and more preferably from 12 to 24 hours.

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The temperature range at which the equilibrium takes place may range from -15 ° C to 75 ° C, and is preferably from 0 ° C to 50 ° C, but more preferably from about 20 ° C to about 30 ° C.

As a result of this balance, they result in at least two fractions, one of which is a contaminant-containing fraction and the other is a substantially purified polydextrose-containing fraction. These fractions may appear as two phases in a container. Formation of the two phases can be accelerated after equilibration by conventional methods used to destabilize emulsions, such as centrifugation, etc. i

Once fractions are formed, for example in the form of layers, the upper layer, which is the contaminant-containing fraction, can be separated by decantation, stored for recovery of the organic solvent, as the upper layer contains mainly solvent, water and low molecular weight polydextrose and flavoring compounds.

The lower layer containing predominantly a purified polydextrose polymer and water is retained and used in the desired form. The pH of the lower layer is about 3.0, and can be adjusted according to different applications. j

Thus, only minimal quantities of salts are required for the product to fine-tune it for the intended use. Bases used to adjust the pH value may include sodium hydroxide, sodium citrate, or potassium hydroxide. In terms of optimizing the aroma of polydextrose, potassium salts should be avoided as potassium ions impair and lead to an undesirable aroma of the product. 0 Residual solvent in the lower phase is easily removed by boiling, evaporating under reduced pressure or other conventional processes. In addition, the lower layer may be dried if necessary to

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obtain a powder by drying under reduced pressure, spray drying and other conventional processes.

The final product is substantially free of aroma compounds which can be determined by sensory evaluation. The amount of flavored compounds; in the product is effected by the initial proportion of polydextrose, water and polar organic solvents. The present invention includes the discovery of a range of proportions of | water to solvent polydextrose which is significantly in carrying out the unexpectedly effective process of the present invention. These interesting results will be explained in combination with the following examples.

EXAMPLES

Samples were prepared using the general procedure described above in a polydextrose to water to solvent ratio as shown in Tables I and II below with respect to ethanol as solvent in Table I and acetone as solvent in Table II.

For example, Lot # 8 of the ethanol-polydextrose-water example was conducted as follows. Type A polydextrose, water and pure ethanol were present in amounts of 30, 20 and 50 parts (w / w) in a flask. Vigorous stirring was applied until an emulsion formed. The emulsion mixture was equilibrated for 18 hours at room temperature and then centrifuged at 1500xg for 10 minutes after equilibration. The supernatant was decanted off by decantation. The lower phase was then heated to remove residual ethanol. The pH value of this end product was approximately 2.5 to 3.0, which was adjustable to accommodate different applications. The polydextrose yield was approximately 70% of the original solids. This end product as indicated in Table I had an acceptable sensory rating of 2.

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Lot number

Ethanol solvent

P / P / P ratio

Polydextrose: Water: Solvent

Degree of

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10:10:80

20:10:70 10:20:70 30:10:60 20:20:60 10:30:60 40:10:50 30:20:50 20:30:50 50:10:40 40:20:40 30:30:40 60:10:30 50:10:40 70:10:20 60:20:20 80:10:10 70:20:10

A scale of 1 - 3 was used for sensory evaluation.

grade 3 represents a product with the best taste quality while grade I represents the worst taste.

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The product prepared according to the sample referred to herein has been tested to taste and given a comparative grade 1 to 3.

Example 8 of the acetone-polydextrose-water combination was processed using Type A polydextrose, water and acetone present in ratios of 30, 20 and 50 parts (w / w / w). The preparation procedure was the same as that set forth in the above Example with respect to ethanol as a solvent. Polydextrose recovery at the end of Lot 8 of approximately 90% of original solids₀ This product had an acceptable sensory rating of 2 as shown in Table II below.

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TABLE II

Acetone Solvent

Lot number

Aspect Ratio (P / P / P)

Polydextrose; Water: Solvent

10:10:80

Degree of sensitivity

20:70:70 2 10:20:70 2 30:10:60 2 20:20:60 2 10:30:60 3 40:10:50 2 30:20:50 2 20:30:50 2 10:40:50 3 50:10:40 1 40:20:40 1 30:30:40 2 60:10:30 1

50:20:301

40:30:301

70:10:201

60:20:201

50:30:2’01

For the ternary phase diagrams the results indicate the optimal proportions of polydextrose, water and ethanol or acetone required for purification of polydextrose to produce an organoleptically acceptable product. In Figures 1a and 2a, the area marked by solid circles indicates proportions where the solvent polydextrose does not separate. The so-called open circle points represent good separation of a polydextrose enriched phase and a solvent enriched phase.

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In Figures 1b and 2b, the areas with the highest rating of 3 show the most preferred range of proportions, while areas where the highest rating of 2 appear show the preferred range of proportions.

According to these extraction conditions, the resulting polydehyde product has little, if any, taste.

It should be noted that polydextrose of

Type N, for example in solution, may also be purified by the procedure of the present invention when the water content is taken into account.

EXAMPLE OF A HARD SWEET

Hard candy samples were prepared using the purified polydextrose according to the present invention. It was especially found that it was easier to bake and handle purified polydextrose in the presence of various low molecular weight compounds that could be added after purification, such compounds behaving as plasticizers in the polymeric matrix.

Specifically, intensive sweeteners may also be used which include those mentioned in the following non-limiting list:

Water-soluble artificial sweeteners such as soluble saccharin salts, i.e. sodium or calcium saccharin, sucralose, cyclamate salts, acesulfam-K and the like, and the free acid form of saccharin. In addition to dipeptide-based sweeteners such as L-aspartyl-L-finylalanine methyl ester and materials described in US Patent 3,492,131 and the like. In general, the amount of sweeteners will vary with the amount of sweetness desired for the particular sweetening be it a chewing gum, a candy or a tablet. Artificial sweeteners described in the above mentioned categories are used in amounts between

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about 0.005 θ about 5.0% and more preferably between about 0.05% and about 2.5% by weight of the final composition.

Suitable flavors include natural and artificial flavors, and mint flavors such as peppermint, spearmint, menthol, artificial vanilla, vanilla, artificial chocolate, chocolate, cinnamon, various individual and mixed fruit flavors and the like. Flavorings are generally used in amounts which vary depending on the individual flavor, and may, for example, vary in amounts from 0.5% to about 3% by weight of the final composition.

The dyes used in the present invention include pigments which may be incorporated in amounts up to 6% by weight of the composition. The preferred pigment, titanium dioxide, may be incorporated in amounts up to 1% by weight. In addition, the dyes may also include other dyes suitable for food, pharmaceutical and cosmetic applications, and are known as FD&amp;G dyes and the like. Acceptable materials in the above spectrum are preferably water soluble. Illustrative examples include indigo blue, known as FD&amp;C blue. NS 2 which is the disodium salt of 5,5-indigotindisulfonic acid. Similarly, the dye known as FD&amp;C green. No. 91, comprises a triphenyl methane dye and is the 4- (N-ethyl-p-sulfobenzylamino) (diphenylmethylene) - (1- (N-ethyl-methyl) salt. Np-sulfoniobenzyl) -2,5-cyclohexadienimine. A complete list of all FD &amp; CeD &amp; Ceas dyes and their corresponding chemical structures can be found in Kirk-Othmer Encyclopedia of Chemical Technology, 38th Edition, Volume 6, on Pages 561-595, which is incorporated herein by reference.

When preparing a hard candy composition, acids such as citric acid, isocitric acid, maleic acid, acid may also be included.

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fumaric acid, succinic acid, adipic acid, malic acid and tartaric acid, with citric acid being preferred.

A real composition was prepared according to the following process. The glycerine purified polydextrose was boiled at 130 ° C. The resulting product was allowed to cool to 80 ° C. Citric acid, sweetener, flavor and colorant were added to the cold product. The resulting product was then placed on a cooling table and processed to evenly distribute the ingredients.

I diente. The product was then formed into hard candy pieces.

FORMULATION

HARD SWEET WITH CHERRY FLAVOR

<td>Ingredient</td><td>P / P</td>

<td>Purified Polydextrose</td><td> 94,0</td>

<td>Glycerin</td><td> 5,0</td>

<td>Citric acid</td><td> 0,5</td>

<td>Aspartame</td><td> 0,2</td>

<td>Aroma</td><td> 0,2</td>

<td>Red color // 40</td><td> 0,1</td>

After rehearsing the hard candy produced!

In accordance with the above procedure, it was found that a product of very good quality and sweetness was obtained which was organoleptically pleasing and also aesthetically acceptable.

Thus, while describing what are currently thought to be preferred embodiments of the invention, those skilled in the art will appreciate that further and additional modifications to the invention may be made without departing from the invention.

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its true scope and is intended to claim all such changes and modifications as falling within the scope of the present invention.