WO1990006061A1

WO1990006061A1 - Method of controlling release of alitame in chewing gum and gum produced thereby

Info

Publication number: WO1990006061A1
Application number: PCT/US1989/001269
Authority: WO
Inventors: Robert J. Yatka
Original assignee: Wm. Wrigley Jr. Company
Priority date: 1989-03-28
Filing date: 1989-03-28
Publication date: 1990-06-14

Abstract

The present invention is a method for producing a chewing gum with a delayed release Alitame sweetener, as well as the chewing gum so produced. The delayed release Alitame sweetener is obtained by physically modifying Alitame's properties by coating and drying. Alitame sweetener is coated by encapsulation, partially coated by agglomeration, entrapped by absorption, or treated by multiple steps of encapsulation, agglomeration, and absorption. The coated sweetener is then co-dried and particle sized to produce a release-modified Alitame high-intensity sweetener. When incorporated into the chewing gum, these particles are adopted to enhance the shelf stability of the sweetener and/or produce a delayed release when the gum is chewed.

Description

METHOD OF CONTROLLING RELEASE OF ALITAME IN CHEWING GUM AND GUM PRODUCED THEREBY

BACKGROUND OF THE INVENTION

The present invention relates to methods for producing chewing gum. More particularly the invention relates to producing chewing gum containing high- potency sweeteners which have been treated to control their release and enhance shelf-life stability.

In recent years, efforts have been devoted to controlling release characteristics of various ingre¬ dients in chewing gum. Most notably, attempts have been made to delay the release of sweeteners and flavors in various chewing gum formulations to thereby lengthen the satisfactory chewing time of the gum. Delaying the release of sweeteners and flavors can also avoid an undesirable overpowering burst of sweetness or flavor during the initial chewing period. On the other hand, some ingredients have been treated so as to increase their rate of release in chewing gum.

In addition, other efforts have been directed at perfecting the use of high-potency sweeteners within the chewing gum formulation, to thereby increase the shelf-life stability of the ingredients, i.e. the pro¬ tection against degradation of the high-potency sweetener over time. One such high-potency sweetener is Alitame (L-α-Aspartyl-N-(2,2,4,4-tetramethyl-3-thietanyl-D-ala- ninamide hydrate) . This sweetener, which is not yet approved for use in food products and chewing gum, is being considered by the FDA as a food additive. The manufacturer of Alitame is the Pfizer Corporation of Groton, Connecticut. This highly consumer-acceptable, high-potency sweetener gives chewing gum a fast, strong release that is not desirable. Methods of treating the high-potency sweetener to delay the release or sweetness in balance with the chewing gum flavor would therefore be a definite improvement.

Use of Alitame in chewing gum has been dis¬ closed in several patents. U.S. Patent 4,411,925 dis¬ closes simple addition of Alitame in gum. U.S. 4,536,396 discloses combinations of Alitame and Acesulfame K in foods including chewing gum.

Other patents disclose how a sweetener like aspartame can be physically modified to control the release rate in chewing gum. For example, U.S. Patent No. 4,597,970 to Sharma et al. teaches a process for producing an agglomerated sweetener wherein the sweetener is dispersed in a hydrophobic matrix consisting essentially of lecithin, a glyceride, and a fatty acid or wax having a melting point between 25°C. and 100°C. The method disclosed uses a spray-congealing step to form the sweetener-containing matrix into droplets, followed by a fluid-bed second coating on the agglomerated particles. U.S. Patent Nos. 4,515,769 and 4,386,106, both to Merrit et al., teach a two step process for preparing a delayed release flavorant for chewing gum. In this process, the flavorant is prepared in an emulsion with a hydrophilic matrix. The emulsion is dried and ground and the particles are then coated with a water-impermeable substance.

U.S. Patent No. 4,230,687 to Sair et al. teaches a process for encasing an active ingredient to achieve gradual release of the ingredient in a product such as chewing gum. The method described involves adding the ingredient to an encapsulating material in the form of a viscous paste. High-shear mixing is used to achieve a homogeneous dispersion of the ingredient within the matrix, which is subsequently dried and ground.

U.S. Patent No. 4,139,639 to Bahoshy et al. teaches a process of "fixing" aspartame by co-drying (by spray drying or fluid-bed coating) a solution con¬ taining aspartame and an encapsulating agent, such as gum arabic, to thereby surround and protect the aspartame in the gum during storage.

U.S. Patent No. 4,384,004 to Cea et al. teaches a method of encapsulating aspartame with various solutions of encapsulating agents using various encapsulation techniques, such as spray drying, in order to increase the shelf-stability of the aspartame.

U.S. Patent No. 4,634,593 to Stroz et al. teaches a method for producing controlled release sweeteners for confections, such as chewing gum. The method taught therein involves the use of an insoluble fat material which is mix mulled with the sweetener. SUMMARY OF INVENTION

The present invention is a method for produc¬ ing chewing gum with a modified high-potency sweetener, specifically Alitame, as well as the chewing gum so produced. The delayed release high-potency sweetener is obtained by modifying the sweetener by encapsula¬ tion, partial encapsulation or partial coating, en¬ trapment or absorption with low water-soluble materials or water-insoluble materials. The procedures for modifying the sweetener include spray drying, spray chilling, fluid-bed coating, coacervation, and other agglomerating and standard encapsulating techniques. The sweetener may also be absorbed onto an inert or water-insoluble material. The sweetener may be modi¬ fied in a multiple step process comprising any of the processes or combination of processes noted. The sweetener, Alitame, may also be combined with other sweeteners including, but not limited to, sucrose, dextrose, fructose, maltose, maltodextin, xylose, pala- tinose, or others that are considered bulk sweeteners, as well as sugar alcohols including but not limited to sorbitol, mannitol, xlitol, maltitol, lactitol, palatinit, and lycasin. The high-potency sweetener Alitame may also be combined with other high-potency sweeteners including, but not limited to, thaumatin, aspartame, sodium saccharin, calcium cyclamate, glycyrrhizin, acesulfame K, sucralose, stevioside and dihydrochalcones.

This sweetener, Alitame, when modified according to the present invention, gives a chewing gum having a controlled-release sweetener. A higher quantity of sweetener can be used without resulting in a high initial sweetness impact, but instead having a delayed sweetness release that is compatible with the delayed flavor release in chewing gum, giving a highly consumer-acceptable chewing gum product.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

Alitame ( -α-Aspartyl-N-(2,2,4,4-tetramethyl- 3-thietanyl-D-alaninamide hydrate) is a new, high- potency sweetener which is about 2000 times sweeter than sugar. The taste properties of Alitame are considered good. At concentrations usually used, Alitame has a pure and rapidly perceptible sweet taste that does not linger.

When Alitame is added to chewing gum at a level of about 0.01%-0.05%, the sweetener gives chewing gum a fast, intense sweetness that dissipates quickly, leaving a strong flavor character that is less pleasant. It would be considered a significant improvement to a chewing gum to have the Alitame sweetener release its sweetness as the flavor in the gum is released, thus balancing the overall taste perception. Tests of Alitame show that the same fast, intense sweetness results from chewing gum whether the Alitame is added as a fine powder or dissolved in water, glycerin, propylene glycol, corn syrup, hydrogenated starch hyrolyzate, or any other compatible aqueous solution.

For aqueous solutions, an emulsifier can also be mixed in the solution with the Alitame sweetener and the mixture added to a chewing gum. A flavor can also be added to the sweetener/emulsifier mixture. Powdered Alitame may also be mixed into a molten chewing gum base during base manufacture or prior to manufacture of the gum. Alitame may also be mixed with base ingredients during base manufacture.

Usage levels of Alitame in water or an aqueous solvent is limited to its solubility in the aqueous solvent. Solubility of Alitame in water is approximately 13g/100 ml at its isoelectric point and 25°C, and increases to 30g/100 ml at 50°C. At both high and low pHs, Alitame has solubilities up to 50% at 50°C. In solvents like ethanol or propylene glycol, solubility of Alitame is very high. Whether as a powder or as an aqueous liquid, the amount of Alitame added to chewing gum is about 0.001% to 1%. Preferably the range of Alitame in gum is about 0.01% to about 0.2%, and more preferably about 0.02% to about 0.05%. Most preferably, the level of Alitame in gum is about 0.03%.

As stated previously, Alitame releases very quickly from chewing gum during the early stages of mastication of the gum because of its high solubility in water. Physical modifications of the sweetener by encapsulation with another substrate will slow its release in chewing gum by reducing the solubility or dissolution rate of Alitame. Any standard technique which gives partial or full encapsulation of the Alitame sweetener can be used. These techniques in¬ clude, but are not limited to, spray drying, spray chilling, fluid-bed coating and coacervation. These encapsulation techniques that give partial encapsula¬ tion or full encapsulation can be used individually or in any combination in a single step process or multiple step process. Generally, delayed release of sweetener is obtained in multistep processes like spray drying the sweetener and then fluid-bed coating of the re¬ sultant powder.

The encapsulation techniques here described are standard coating techniques and generally give varying degrees of coating from partial to full coat¬ ing, depending on the coating composition used in the process. Also, the coating compositions may be suscep¬ tible to water permeation to various degrees. Gener¬ ally, compositions that have high organic solubility, good film-forming properties and low water solubility give better delayed release of the sweetener. Such compositions include acrylic polymers and copolymers, carboxyvinyl polymer, polyamides, polystyrene, poly- vinyl acetate, polyvinyl acetate phthalate, polyvinyl- pyrrolidone, and waxes. Although all of these ma¬ terials are possible for encapsulation of Alitame sweetener, only food-grade materials should be con¬ sidered. Two standard food-grade coating materials that are good film formers but not water soluble are shellac and Zein. Others which are more water soluble, and good film formers, are materials like agar, algi- nates, a wide range of cellulose derivatives like ethyl cellulose, methyl cellulose, sodium hydroxymethyl cellulose, and hydroxypropylmethyl cellulose, dextrin, gelatin, and modified starches. These ingredients, which are generally approved for food use, also give a delayed release when used as an encapsulant for Alitame. Other encapsulants like acacia or malto- dextrin can also encapsulate Alitame, but give very little change in the release rate of Alitame in gum.

The amount of coating or encapsulating material on the sweetener Alitame also controls the length of time for its release from chewing gum. Generally, the higher the level of coating and the lower the amount of active Alitame, the slower the release of the sweetener during mastication. The release rate is generally not instantaneous, but gradual over an extended period of time. To obtain the desired sweetness release to blend with a gum's flavor release, the encapsulant should be a minimum of about 20% of the coated sweetener. Preferably, the encap¬ sulant should be a minimum of about 30% of the coated sweetener, and most preferably should be a minimum of about 40% of the coated sweetener. Depending on the coating material, a higher or lower amount of coating material may be needed to give the desired release of sweetener to balance sweetness release with flavor release.

Another method of giving a delayed release of the sweetener, Alitame, is agglomeration of the sweetener with an agglomerating agent which partially coats the sweetener. This method includes the step of mixing the sweetener and agglomerating agent with a small amount of water or solvent. The mixture is pre¬ pared in such a way as to have individual wet particles in contact with each other so a partial coating can be applied. After the water or solvent is removed, the mixture is ground and used as a powdered, coated sweetener.

Materials that can be used as the agglomera¬ ting agent are the same as those used in encapsulation mentioned previously. However, since the coating is only a partial encapsulation and the Alitame sweetener is very water soluble, some agglomerating agents are more effective in delaying the sweetener release than others. Some of the better agglomerating agents are the organic polymers like acrylic polymers and co- polymers, polyvinyl acetate, polyvinylpyrrolidone, waxes, shellac, and Zein. Other agglomerating agents are not as effective in giving the sweetener a delayed release as are the polymers, waxes, shellac and Zein, but can be used to give some delayed release. These other agglomerating agents include, but are not limited to, agar, alginates, a wide range of cellulose deriva- tives like ethyl cellulose, methyl cellulose, sodium hydroxymethyl cellulose, hydroxypropylmethyl cellulose, dextrin, gelatin, modified starches, and vegetable gums like guar gum, locust bean gum, and carrageenin. Even though the agglomerated sweetener is only partially coated, when the quantity of coating is increased com¬ pared to the quantity of Alitame sweetener, the release of the sweetener can be delayed for a longer time during mastication. The level of coating used in the agglomerated product is a minimum of about 5%. Prefer¬ ably the coating level is a minimum of about 15% and more preferably about 20%. Depending on the agglomer¬ ating agent, a higher or lower amount of agent may be needed to give the desired release of sweetener to balance sweetness release with flavor release.

The Alitame sweetener may be coated in a two-step process or multiple step process. The sweetener may be encapsulated with any of the materials as described previously and then the encapsulated sweetener can be agglomerated as described previously to obtain an encapsulated/agglomerated/sweetener product that could be used in chewing gum to give a delayed release of sweetener.

In another embodiment of this invention, Alitame sweetener may be absorbed onto another com¬ ponent which is porous, thus becoming entrapped in the matrix of the porous component. Common materials used for absorbing the sweetener include, but are not limited to, silicas, silicates, pharmasorb clay, spongelike beads or microbeads, amorphous sugars like dried dextrose, sucrose, alditols, amorphous carbonates and hydroxides, including aluminum and calcium lakes, vegetable gums and other spray dried materials.

Depending on the type of absorbant material and how it is prepared, the amount of Alitame sweetener that can be loaded onto the absorbant will vary. Generally materials like polymers or sponglike beads or microbeads, amorphous sugars and alditols and amorphous carbonates and hydroxides absorb about 10% to about 40% of the weight of the absorbant. Other materials like silicas and pharmasorb clays may be able to absorb about 20% to about 80% of the weight of the absorbant.

The general procedure for absorbing the sweetener onto the absorbent is as follows. An absorbent like fumed silica powder can be mixed in a powder blender and an aqueous solution of the Alitame sweetener can be sprayed onto the powder as mixing continues. The aqueous solution can be about 5% to 30% Alitame solids, and higher solid levels may be used if temperatures up to 90°C are used. Generally water is the solvent, but other solvents like alcohol could also be used if approved for use in food. As the powder mixes, the liquid is sprayed onto the powder. Spraying is stopped before the mix becomes damp. The still flowing powder is removed from the mixer and dried to remove the water or other solvent, and ground to a spe¬ cific particle size.

After the Alitame sweetener is absorbed onto an absorbant or fixed onto an absorbant, the fixative/ sweetener can be coated by encapsulation. Either full or partial encapsulation may be used, depending on the coating composition used in the process. Full en¬ capsulation may be obtained by coating with a polymer as in spray drying, spray chilling, fluid-bed coating, coacervation, or any other standard technique. A partial encapsulation or coating can be obtained by agglomeration of the fixative/sweetener mixture using any of the materials discussed above.

The three methods of use to obtain a delayed release of Alitame sweetener are: (1) encapsulation by spray drying, fluid-bed coating, spray chilling and coacervation to give full or partial encapsulation, (2) agglomeration to give partial encapsulation and (3) fixation or entrapment/absorption which also gives partial encapsulation. These three methods, combined in any usable manner which physically isolates the Alitame sweetener, reduces its dissolvability or slows down the release of sweetener, are included in this in¬ vention.

Other methods of treating the Alitame sweetener to physically isolate the sweetener from other chewing gum ingredients may also have some effect on its release rate and stability. The Alitame sweetener may be added to the liquid inside a liquid center gum product. The center fill of a gum product may comprise one or more carbohydrate syrups, glycerin, thickeners, flavors, acidulants, colors, sugars and sugar alcohols in conventional amounts. The ingre¬ dients are combined in a conventional manner. The Alitame sweetener is dissolved in the center-fill liquid and the amount of Alitame sweetener added to the center-fill liquid is about 5 ppm to about 400 ppm by weight of the entire chewing gum formula. This method of using Alitame sweetener in chewing gum can allow for a lower usage level of the sweetener, can give the sweetener a smooth release rate, and can reduce or eliminate any possible reaction of the sweetener with gum base, flavor components or other components, yield¬ ing improved shelf stability.

Another method of isolating Alitame sweetener from other chewing gum ingredients is to add Alitame to the dusting compound of a chewing gum. A rolling or dusting compound is applied to the surface of chewing gum as it is formed. This rolling or dusting compound serves to reduce sticking to machinery as it is formed, reduces sticking of the product to machinery as it is wrapped, and sticking to its wrapper after it is wrapped and being stored. The rolling compound com¬ prises Alitame sweetener in combination with mannitol, sorbitol, sucrose, starch, calcium carbonate, talc, other orally acceptable substances or a combination thereof. The rolling compound constitutes from about 0.25% to about 10.0%, but preferably about 1% to about 3% of weight of the chewing gum composition. The amount of Alitame sweetener added to the rolling com¬ pound is about 0.01% to about 20% of the rolling com¬ pound or about 1 ppm to about 2000 ppm of the chewing gum composition. This method of using Alitame sweetener in the chewing gum can allow a lower usage level of the sweetener, can give the sweetener a more controlled release rate, and can reduce or eliminate any possible reaction of the sweetener with gum base, flavor components, or other components, yielding im¬ proved shelf stability.

Another method of isolating Alitame sweetener is to use it in the coating/panning of a pellet chewing gum. Pellet or ball gum is prepared as conventional chewing gum, but formed into pellets that are pillow shaped or into balls. The pellets/balls can be then sugar coated or panned by conventional panning techniques to make a unique sugar coated pellet gum. Alitame sweetener is very stable and highly water soluble, and can be easily added to a sugar solution prepared for sugar panning. Alitame can also be added as a powder blended with other powders often used in some types of conventional panning procedures. Using Alitame sweetener isolates the sweetener from other gum ingredients and modifies its release rate in chewing gum. Levels of use of Alitame may be about 10 ppm to about 500 ppm in the coating and about 5 ppm to about 200 ppm of the weight of the chewing gum product. The weight of the coating may be about 20% to about 50% of the weight of the finished gum product.

Conventional panning procedures generally coat with sucrose, but recent advances in panning have allowed the use of other carbohydrate materials to be used in the place of sucrose. Some of these components include, but are not limited to, dextrose, maltose, palatinose, xylitol, lactitol, palatinit and other new additols or a combination thereof. These materials may be blended with panning modifiers including, but not limited to, gum arabic, maltodextrins, corn syrup, gelatin, cellulose type materials like carboxymethyl cellulose, or hydroxymethyl cellulose, starch and modified starches, vegetable gums like alginates, locust bean gum, guar gum, and gum tragacanth, in¬ soluble carbonates like calcium carbonate or magnesium carbonate and talc. Antitack agents may also be added as panning modifiers which allow the use of a variety of carbohydrates and sugar alcohols to be used in the development of new panned or coated gum products. Flavors may also be added with the sugar coating and with the Alitame sweetener to yield unique product characteristics.

Another type of pan coating would also isolate the Alitame sweetener from the chewing gum in¬ gredients. This technique is referred to as film coat¬ ing and is more common in pharmaceuticals than in chew¬ ing gum, but procedures are similar. A film like shellac, Zein, or cellulose-type material is applied onto a pellet-type product forming a thin film on the surface of the product. The film is applied by mixing the polymer, a plasticizer and a solvent (pigments are optional) and spraying the mixture onto the pellet sur- face. This is done in conventional type panning equip¬ ment, or in more advanced side-vended coating pans. When a solvent like alcohol is used, extra precautions are needed to prevent fires and explosions, and specialized equipment must be used. Since Alitame is highly soluble in alcohol, solvent films can be added that contain the Alitame sweetener. This will give a unique sweetness release to a film coated product.

Some film polymers can use water as the solvent in film coating. Recent advances in polymer research and in film coating technology eliminates the problem associated with the use of solvents in coating. These advances make it possible to apply aqueous films to a pellet or chewing gum product. As Alitame sweetener is highly water soluble, it can be added to this aqueous film solution and applied with the film to the pellet or chewing gum product. The aqueous film or even the alcohol solvent film may also contain a flavor along with the polymer and plasticizer. By adding Alitame sweetener to the polymer/plasticizer/solvent system either as an emulsion or solution, the sweetener can add sweetness to the flavor and a balanced flavor/ sweetness can be obtained. The Alitame sweetener can also be dissolved in the aqueous solvent and coated on the surface with the aqueous film. This will give a unique sweetness release to a film coated product.

The previously described encapsulated, ag¬ glomerated, or absorbed high-potency sweetener may readily be incorporated into a chewing gum composition. The remainder of the chewing gum ingredients are non- critical to the present invention. That is, the coated particles of high-potency sweetener can be incorporated into conventional chewing gum formulations in a con¬ ventional manner. Naturally, the preferred chewing gum formulation is a sugarless chewing gum. However, the high-potency sweeteners may also be used in a sugar chewing gum to intensify and/or extend the sweetness thereof. The coated high-potency sweetener may be used in either regular chewing gum or bubble gum.

In general, a chewing gum composition typic¬ ally comprises a water-soluble bulk portion, a water- insoluble chewable gum base portion and typically water-insoluble flavoring agents. The water-soluble portion dissipates with a portion of the flavoring agent over a period of time during chewing. The gum base portion is retained in the mouth throughout the chew.

The insoluble gum base generally comprises elastomers, resins, fats and oils, waxes, softeners and inorganic fillers. Elastomers may include polyisobuty- lene, isobutylene-isoprene copolymer and styrene butadiene rubber, as well as natural latexes such as chicle. Resins include polyvinylacetate and terpene resins. Fats and oils may also be included in the gum base, including tallow, hydrogenated and partially hydrogenated vegetable oils, and cocoa butter. Com¬ monly employed waxes include paraffin, microcrystalline and natural waxes such as beeswax and carnauba. Ac¬ cording to the preferred embodiment of the present in¬ vention, the insoluble gum base constitutes between about 5 to about 95 percent by weight of the gum. More preferably the insoluble gum base comprises between 10 and 50 percent by weight of the gum and most preferably about 20 to about 35 percent by weight of the gum.

The gum base typically also includes a filler component. The filler component may be calcium carbonate, magnesium carbonate, talc, dicalcium phosphate or the like. The filler may constitute between about 5 and about 60 percent by weight of the gum base. Preferably, the filler comprises about 5 to about 50 percent by weight of the gum base.

Gum bases typically also contain softeners, including glycerol monostearate and glycerol tri¬ acetate. Further, gum bases may also contain optional ingredients such as antioxidants, colors, and emulsi- fiers. The present invention contemplates employing any commercially acceptable gum base.

The water-soluble portion of the chewing gum may further comprise softeners, sweeteners, flavoring agents and combinations thereof. Softeners are added to the chewing gum in order to optimize the chewability and mouth feel of the gum. Softeners, also known in the art as plasticizers or plasticizing agents, gener¬ ally constitute between about 0.5 to about 15.0 percent by weight of the chewing gum. Softeners contemplated for use in the present invention include glycerin, lecithin, and combinations thereof. Further, aqueous sweetener solutions such as those containing sorbitol, hydrogenated starch hydrolysates, corn syrup and combinations thereof may be used as softeners and binding agents in gum.

As mentioned above, the coated high-potency sweeteners of the present invention will most likely be used in sugarless gum formulations. However, formula¬ tions containing sugar are also within the scope of the invention. Sugar sweeteners generally include saccharide- containing components commonly known in the chewing gum art which comprise, but are not limited to, sucrose, dextrose, maltose, dextrin, dried invert sugar, fructose, levulose, galactose, corn syrup solids and the like, alone or in any combination.

The coated high-potency sweeteners of the present invention can also be used in combination with other sugarless sweeteners. Generally sugarless sweeteners include components with sweetening charac¬ teristics but which are devoid of the commonly known sugars and comprise, but are not limited to, sugar alcohols such as sorbitol, mannitol, xylitol, hydro¬ genated starch hydrolysates, maltitol and the like, alone or in any combination.

Depending on the particular sweetness release profile and shelf-stability needed, the coated high- potency sweeteners of the present invention can also be used in combination with uncoated high-potency sweeteners or with high-potency sweeteners coated with other materials and by other techniques.

A flavoring agent may be present in the chew¬ ing gum in an amount within the range of from about 0.1 to about 10.0 weight percent and preferably from about 0.5 to about 3.0 weight percent of the gum. The flavoring agents may comprise essential oils, synthetic flavors, or mixture thereof including, but not limited to, oils derived from plants and fruits such as citrus oils, fruit essences, peppermint oil, spearmint oil, clove oil, oil of wintergreen, anise, and the like. Artificial flavoring components are also contemplated for use in gums of the present invention. Those skilled in the art will recognize that natural and artificial flavoring agents may be combined in any sensorally acceptable blend. All such flavors and flavor blends are contemplated by the present in¬ vention.

Optional ingredients such as colors, emulsi- fiers and pharmaceutical agents may be added to the chewing gum.

In general, chewing gum is manufactured by sequentially adding the various chewing gum ingredients to a commercially available mixer known in the art. After the ingredients have been thoroughly mixed, the gum mass is discharged from the mixer and shaped into the desired form such as by rolling into sheets and cutting into sticks, extruding into chunks or casting into pellets.

Generally, the ingredients are mixed by first melting the gum base and adding it to the running mixer. The base may also be melted in the mixer it¬ self. Color or emulsifiers may also be added at this time. A softener such as glycerin may also be added at this time, along with syrup and a portion of the bulk¬ ing agent. Further portions of the bulking agent may then be added to the mixer. A flavoring agent is typically added with the final portion of the bulking agent. The coated sweetener of the present invention is preferably added after the final portion of bulking agent and flavor have been added.

The entire mixing procedure typically takes . from five to fifteen minutes, but longer mixing times may sometimes be required. Those skilled in the art will recognize that many variations of the above de¬ scribed procedure may be followed.

Examples

The following examples of the invention and comparative examples are provided by way of explanation and illustration.

The formulas listed in Table 1 comprise various sugar-free formulas in which Alitame can be added to gum after it is dissolved in various solvents. TABLE 1

(Wt . %)

In Example 1, Alitame powder was added directly to the gum.

In Example 2, a 5.0 g portion of Alitame was dissolved in 45.0 g water, making a 10.0% solution, and added to gum.

In Example 3, a 2.0 gram portion of Alitame was dissolved in 98.0 gram propylene glycol, making a 2.0% solution, and added to gum.

In Example 4, a 2.0 gram portion of Alitame was dissolved in 98.0 gram of glycerin, making a 2% solution, and added to gum. In Example 5, a 2.0 gram portion of Alitame was dissolved in hot hydrogenated starch hydrolysates, making a 2% solution, and added to gum.

In the next examples of a sugar gum formula¬ tion, Alitame can be dissolved in water and emulsifiers and added to the aqueous solution. Example solutions can be prepared by dissolving 10 grams of Alitame in 90 grams water and adding 10 grams of emulsifiers of various hydrophilic-lipophilic balance (HLB) values to the solution. The mixtures can then be used in the following formulas.

TABLE 2 ( t. %)

Examples 12-16 - The same as the formulations made in Examples 6-11, respectively, except that the flavor can be mixed together with the aqueous sweetener solution and emulsified before adding the mixture to the gum batch.

Alitame sweetener can also be blended into various base ingredients. A typical base formula is as follows:

100%

The individual base components can be softened prior to their addition in the base manufacturing process. To the presoftened base component, Alitame can be added and mixed, and then the presoftened base/sweetener blend can be added to make the finished base. In the following examples, Alitame can be mixed first with one of the base ingredients, and the mixed ingredient can then be used in making a base. The ingredients blended with Alitame can then be used at the levels indicated in the typical base formula above.

Example 17 - The terpene resin used to make the base can be 99.6% polyterpene resin and 0.4% Alitame.

Example 18 - The polyvinyl acetate used to make the base can be 99.6% low M.W. polyvinyl acetate and 0.4% Alitame. Example 19 - The paraffin wax used to make the base can be 99.2% paraffin wax and 0.8% Alitame.

The Alitame may also be added to an otherwise complete gum base.

Example 20 - 0.1% Alitame can be mixed with 99.9% of a gum base have the above listed typical formula. The Alitame can be added near the end of the process after all the other ingredients are added.

The samples of finished base made with

Alitame added to different base components can then be used in a sugar-type chewing gum formulated as follows:

TABLE 3 (Wt, % )

(For examples 17, 18, 19, and 20)

Sugar 55.2

Base 19.2

Corn Syrup 13.4

Glycerine 1.4

Dextrose

Monohydrate 9.9

Peppermint

Flavor 0.9

100%

The theoretical level of Alitame sweetener is 0.02% in the finished gum.

Using the following formulation of a sugar- free gum, a variety of encapsulated Alitame samples can be used:

For spray drying, the solids level of an aqueous or alcoholic solution can be about 10-50%, but preferred levels are indicated in the examples listed.

Example 22 - An 80% shellac, 20% active Alitame powder mixture is obtained by spray drying an alcohol/shellac/Alitame emulsion at total solids of 25%.

Example 23 - A 50% shellac, 50% active Alitame powder mixture is obtained by spray drying an appropriate ratio of alcohol/shellac/Alitame emulsion at 25% solids.

Example 24 - A 70% Zein, 30% active Alitame powder mixture is obtained by spray drying an alcohol/ Zein/Alitame emulsion at 30% solids.

Example 25 - A 40% shellac, 60% Active Alitame powder mixture is obtained by fluid-bed coating Alitame with an alcohol/shellac solution at 20% solids.

Example 26 - A 60% shellac, 40% active Alitame powder mixture is obtained by fluid-bed coating Alitame with an alcohol/shellac solution of 25% solids.

Example 27 - A 40% Zein, 60% active Alitame powder mixture is obtained by fluid-bed coating Alitame with an alcohol/Zein solution of 25% solids.

Example 28 - An 85% wax, 15% active Alitame powder mixture is obtained by spray chilling a mixture of molten wax and Alitame.

Example 29 - A 70% wax, 30% active Alitame powder mixture is obtained by spray chilling a mixture of molten wax and Alitame.

Example 30 - A 30% Zein, 70% active Alitame powder mixture is obtained by spray drying an aqueous mixture of Alitame and Zein dispersed in an aqueous, high-pH (pH of 11.6-12.0) media at 15% solids.

Example 31 - A 30% Zein, 70% active Alitame powder mixture is obtained by fluid-bed coating Alitame with a an aqueous, high-pH (pH=11.6-12.0) Zein dis¬ persion of 15% solids.

Example 32 - A 20% Zein, 20% shellac, 60% active Alitame powder mixture is obtained by spray drying an alcohol/shellac/Alitame mixture and then fluid-bed coating the spray dried product for a second coating of alcohol and Zein.

Examples 22 to 32 would all give nearly com¬ plete encapsulation and would delay the release of Alitame sweetener when used in the sugarless gum formulation of Table 4. The higher levels of coating would give a longer delayed release of sweetener than the lower levels of coating. Other polymers that are more water soluble and used in coating would have less of an effect of delaying the release of the Alitame sweetener.

Example 33 - An 80% gelatin, 20% active Alitame powder mixture is obtained by spray drying a gelatin/Alitame solution at 30% solids.

Example 34 - A 30% hydroxypropylmethyl cellu¬ lose (HPMC), 70% Alitame powder mixture is obtained by fluid-bed coating Alitame with an aqueous solution of HPMC at 10% solids.

Example 35 - A 30% carboxymethyl cellulose, 70% active Alitame powder mixture is obtained by fluid bed coating Alitame with an aqueous solution of carboxy methyl cellulose at 10% solids.

Example 36 - A 50% maltodextrin, 50% active Alitame powder mixture is obtained by spray drying an aqueous solution of Alitame and maltodextrin at 40% solids.

Example 37 - A 40% gum arabic, 60% active Alitame powder mixture is obtained by fluid-bed coating Alitame with an aqueous solution of gum arabic at 40% solids.

The coated Alitame from Examples 33, 34 and 35, when used in the chewing gum formula of Table 4, would give a delayed release of sweetener. However, this delayed release would not be extended as much as in the previous examples (22-32), but would show some delayed release compared to the use of Alitame added directly to gum. The product coated with maltodextrin and gum arabic in Examples 36 and 37, when used in the gum formula of Table 4, would show no delay in sweetener release in chewing gum compared to Alitame added directly.

Alitame could also be used in gum as an agglomerated sweetener to give delayed sweetness release. Agglomerated sweeteners can be prepared as in the following examples:

Example 38 - A 15% hydroxypropylmethyl cellu¬ lose (HPMC), 85% active Alitame powder mixture is prepared by agglomerating Alitame and HPMC blended together, with water being added, and the resulting product being dried and ground.

Example 39 - A 15% gelatin, 85% active Alitame powder mixture is made by agglomerating Alitame and gelatin blended together, with water being added, and the resulting product being dried and ground.

Example 40 - A 10% Zein, 90% active Alitame powder mixture is made by agglomerating Alitame with an alcohol solution containing 25% Zein, and drying and grinding the resulting product.

Example 41 - A 15% shellac, 85% active Alitame powder mixture is made by agglomerating Alitame with an alcohol solution containing 25% shellac, and drying and grinding the resulting product.

Example 42 - A 20% HPMC, 80% active Alitame powder mixture is obtained by agglomerating an HPMC and Alitame mixture blended together, with water being added, and the resulting product being dried and ground.

Example 43 - A 20% Zein, 80% active Alitame powder mixture is obtained by agglomerating Alitame and Zein dissolved in high-pH water (11.6-12.0) at 15% solids, with the resulting product being dried and ground.

Example 44 - A 20% wax, 80% active Alitame powder mixture is obtained by agglomerating Alitame and molten wax, and cooling and grinding the resulting product.

Example 45 - A 15% maltodextrin, 85% active Alitame powder mixture is obtained by agglomerating a blend of Alitame and maltodextrin, then adding water, drying and grinding.

All of the above mixtures can be added to any of the following types of chewing gum formulas:

(a) liquid sorbitol (70% sorbitol, 30% water)

(b) hydrogenated starch hydrolyzate syrup

If each of the examples of agglomerated material (38-45) were evaluated in the formulations shown in Table 5, all samples except Example 45 with maltodextrin would give Alitame a delayed release. Samples using Zein, wax, and shellac would give the slowest release rate, whereas samples with HPMC and gelatin would give the next slowest release. Malto¬ dextrin would give a release similar to the release rate of non-coated Alitame added directly to gum as a powder or liquid.

Partially coated or fully coated Alitame can also be used in sugar type gum formulations containing other sugars, such as in the following formulations A-G:

TABLE 6

These formulations may also contain sugar alcohols such as sorbitol, mannitol, xylitol, lactitol, maltitol, palatinit, and lycasin or combinations there- of. Sugarless type gum formulations with partially coated or fully coated Alitame can also be made using various sugar alcohols, such as the following formula¬ tions H-O:

a)

(a) lycasin, all others use sorbitol liquid

All of these formulations in Table 6 and Table 7 which use the agglomerated Alitame as described in the examples (38-45) and in the previous encapsul¬ ated examples (22-35) would be expected to give a delayed release of sweetness compared to a product made by adding Alitame directly to gum as a powder or as liquid.

Multiple step agglomeration/encapsulation procedures can also be used in making release-modified sweetners for use in the formulations in Tables 5, 6 and 7. Examples of multiple step treatments can be prepared as here described:

Example 46 - Alitame is spray dried with maltodextrin at 30% solids to prepare a powder. This powder is then agglomerated with a hydroxypropylmethyl cellulose (HPMC) in a ratio of 85/15 powder/HPMC, wetted with water and dried. After grinding the resulting powder will contain about 68% active Alitame, 17% maltodextrin and 15% HPMC.

Example 47 - Alitame is agglomerated with HPMC in a ratio of 85/15 sweetener HPMC. After drying and grinding, the resulting powder is fluid-bed coated with an alcohol shellac solution at about 25% solids to give a final product containing about 60% active Alitame, 10% HPMC, and about 30% shellac.

Example 48 - Alitame is agglomerated with HPMC in a ratio of 85/15 Sweetener/HPMC. After drying and grinding, the resulting powder is agglomerated with a 15% solids, high-pH, aqueous solution of Zein to give a final product containing about 60% active Alitame, 10% HPMC, and 30% Zein.

Example 49 - Alitame is spray dried with a 25% solution of gelatin. The spray dried product is then agglomerated with a 15% solids, high-pH, aqueous solution of Zein. The final product will contain about 50% active Alitame, 20% gelatin, and 30% Zein.

Example 50 - Alitame is agglomerated with molten wax in a ratio of 85/15 sweetener/wax. When the mixture cools and is ground, it is fluid-bed coated with a 25% Zein - 75% alcohol solution, giving a final product containing 60% active Alitame, 10% wax and 30% Zein. These examples 46-50, when used in any of the formulations noted in Tables 5, 6, and 7 above, will give Alitame a delayed release and delayed sweetness. These multiple step procedures can actually give more delayed release then the single step processes. Mul¬ tiple step processes of more than two steps may give even longer delayed release times, but may generally become less cost effective and less efficient. Prefer¬ ably spray drying can be the first step with additional steps of fluid-bed coating, spray chilling and agglo¬ meration being part of the latter steps.

For absorption type examples, delayed release of Alitame sweetener is dependent on the type of absorbing material. Most materials like silicas, silicates, cellulose, carbonates, and hydroxides would be expected to give a more delayed release than amorphous sugar and sugar alcohols. Some examples that can be prepared are:

Example 51 - A hot 25% solution of Alitame is sprayed onto a precipitated silica to absorb the sweetener. The mixture is dried and coated with a fumed silica. The final product is about 30% active

Alitame.

Example 52 - A hot 25% solution of Alitame is sprayed onto a pharmasorb clay to absorb the sweetener.

The mixture is dried and ground and gives a final product of about 80% clay and 20% active Alitame.

Example 53 - A hot 25% solution of Alitame is sprayed onto a microcrystalline cellulose powder to absorb the sweetener. The mixture is dried and ground and gives a product that is about 70% microcrystalline cellulose and 30% active Alitame.

Example 54 - A hot 25% solution of Alitame is sprayed onto a high absorption starch to absorb the sweetener. The mixture is dried and ground and gives a product that is about 80% starch and 20% active Alitame.

Example 55 - A hot 25% solution of Alitame is sprayed onto a calcium carbonate powder to absorb the sweetener. The mixture is dried and ground and gives a product of about 90% calcium carbonate and 10% active Alitame.

Example 56 - A hot 25% solution of Alitame is sprayed onto a highly absorptive dextrose material to absorb the sweetener. The mixture is dried and ground and gives a product of about 80% dextrose and 20% active Alitame.

Example 57 - A hot 25% solution of Alitame is sprayed onto a sorbitol powder to absorb the material. The mixture is dried and ground and gives a product of about 90% sorbitol and 10% active Alitame.

The samples prepared in examples 51-57 can be used in gum formulations as noted in Tables 5, 6, and 7. Those preparations which have Alitame absorbed onto a material that is not water soluble are expected to give a delayed release of Alitame sweetener.

Another modification or absorption technique may be to dry the Alitame together with a sugar or sugar alcohol, or resolidify the sweetener with sugar or sugar alcohol after both are mixed together in a molten state.

Example 58 - Molten Alitame is added to molten sorbitol in a ratio of 90 parts sorbitol to 10 parts Alitame. The blend is cooled and ground.

Example 59 - Molten Alitame is added to molten dextrose in a ratio of 90 parts dextrose to 10 parts Alitame. The blend is cooled and ground. Example 60 - 4% Alitame is dissolved in 96% high fructose corn syrup. The mixture is evaporated to a low moisture and ground.

The product of examples 58-60 may be added to the gum formulations shown in Tables 5, 6 and 7.

Many of the examples listed are single step processes. However, more delayed release of the Alitame sweetener may be obtained by combining the various processes of encapsulation, agglomeration, ab¬ sorption, and entrappment. Any of the preparations made in Examples 51-60 can be further treated in fluid-bed coating, spray chilling, or coacervation processes to encapsulate the product, and can be agglomerated with various materials and procedures in a variety of multiple step processes.

The Alitame sweetener can also be used with a variety of other high-intensity sweeteners and blended together before encapsulation, agglomeration, absorp¬ tion, and entrappment. Some examples that can be made are:

Example 61 - Alitame and aspartame are blended together in a 1/9 ratio as a powder. This mixture is then spray chilled with wax in a ratio of 70/30 mixture/wax to obtain a powder containing 7% Alitame, 63% aspartame, and 30% wax.

Example 62 - Alitame and thaumatin in a 1/1 ratio are dissolved in water with a 30% solution of gelatin and spray dried. This spray dried powder is then agglomerated with a high-pH aqueous 15% Zein solution. The mixture is dried and ground and gives a product containing 25% Alitame, 25% thaumatin, 35% gelatin, and 15% Zein.

Example 63 - Acesulfame K and Alitame in a 9/1 ratio are prepared in a hot 25% solution. This solution is sprayed onto a high absorption silica powder. The mixture is dried, ground and fluid-bed coated with an alcohol/shellac mixture, giving a product that contains 36% Acesulfame K, 4% Alitame, 40% silica, and 20 % shellac.

Example 64 - Alitame and sucralose in a 1/3 ratio are blended together as a powder and then agglo¬ merated with water and hydroxypropylmethyl cellulose (HPMC) . This blend is dried, ground and agglomerated further with a high-pH, aqueous 15% solution of Zein to obtain a product containing 17% Alitame, 51% sucralose, 12% HPMC and 20% Zein.

Example 65 - Alitame and glycyrrhizin in a 1/9 ratio are blended together as a powder and fluid-bed coated with a solution of 25% shellac in alcohol. The coated product is agglomerated further with water and hydroxypropylmethyl cellulose (HPMC) to obtain a product containing 6% Alitame, 54% glycyrrhizin, 25% shellac, and 15% HPMC.

If the blends of Alitame and other high- intensity sweetners of Examples 61-65 were tested in gum formulations such as those noted in Tables 4, 5, 6 and 7, a significant delayed release of the sweetener and sweetness would be expected. This delayed release would improve the quality of flavor giving it the impression of a longer lasting flavor. Due to the synergistic effects of some of the sweetener combinations in Examples 61-65, less total sweetener may be used to give the same sweetness level as the single delayed release Alitame sweetener.

Alitame can also be combined with other high intensity sweeteners without encapsulation, agglom¬ eration, or absorption and used in chewing gum, as in the following examples: Example 66 -A combination of Altame and aspartame can be used in the formulas listed in Tables 5, 6, and 7 by adjusting the formulas to contain 0.01% Altiame and 0.09% aspartame.

Example 67 - A combination of Alitame and thaumatin can be used in the formulas listed in Tables 5, 6, and 7 by substituting a 1/1 ratio of Alitame to thaumatin for the active blend of Alitame.

Example 68 - A combination of Alitame and sucralose can be used in the formulas listed in Tables 5, 6, and 7 by adjusting the formulas to contain 0.01% Alitame and 0.03% sucralose.

Example 69 - A combination of Alitame and Acesulfame K can be used in the formulas listed in Tables 5, 6, and 7 by adjusting the formulas to contain 0.01% Alitame and 0.09% Acesulfame K.

Example 70 - A combination of Alitame and glycyrrhizin can be used in the formulas listed in Tables 5, 6, and 7 by adjusting the formulas to contain 0.01% Alitame and 0.09% glycyrrhizin.

The formulations of Examples 67-70 do not give a delayed release reaction except for those sweeteners which normally have a slow release. Some of these sweetener combinations may be synergistic, in which case less total sweetener may be needed to give the same sweetness level as a single sweetener.

Claims

I CLAIM:

1. A method for producing chewing gum with Alitame comprising the steps of: a) mixing a quantity of Alitame with a spray drying solvent and an encapsulating material; b) spray drying the mixture in such a way as to encapsulate the Alitame and c) adding a quantity of the spray dried material to a chewing gum formulation to provide an Alitame level in the gum of from 0.005% to 0.1%.

2. The method of Claim 1 wherein the solvent is selected from the group consisting of alcohol and water.

3. The method of Claim 1 wherein the encapsul¬ ating material is selected from the group consisting of shellac and Zein.

4. The method in Claim 1 wherein an additional high-potency sweetener selected from the group consist¬ ing of aspartame, salts of Acesulfame, sucralose, saccharin and its salts, cyclamic acid and its salts, thaumatin, monellin, dihydrochalcone, and combinations thereof is mixed in the spray drying mixture in com¬ bination with the Alitame.

5. A chewing gum made according to the method of Claim 1,

6. A method for producing chewing gum with Alitame comprising the steps of: a) fluid-bed coating Alitame with a solu¬ tion of an encapsulating material and a solvent; b) drying said fluid-bed coated material and c) adding a quantity of the fluid-bed coated material to a chewing gum formulation to provide an Alitame level in the gum formulation of from about 0.005% to about 0.10%.

7. The method of Claim 6 wherein the solvent is selected from the group consisting of alcohol and water.

8. The method of Claim 6 wherein the encapsula¬ ting material is selected from the group consisting of shellac and Zein.

9. The method in Claim 6 wherein an additional high-potency sweetener selected from the group consist¬ ing of aspartame, salts of Acesulfame, sucralose, saccharin and its salts, cyclamic acid and its salts, thaumatin, monellin, dihydrochalcone, and combinations thereof is mixed in the spray drying mixture in com¬ bination with the Alitame.

10. A chewing gum made according to the method of Claim 6.