CA1039567A - Low calorie sweetening composition and method for marking same - Google Patents
Low calorie sweetening composition and method for marking sameInfo
- Publication number
- CA1039567A CA1039567A CA206,437A CA206437A CA1039567A CA 1039567 A CA1039567 A CA 1039567A CA 206437 A CA206437 A CA 206437A CA 1039567 A CA1039567 A CA 1039567A
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- sucrose
- spray
- powder
- bulk density
- solution
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Abstract
ABSTRACT OF THE DISCLOSURE
Readily soluble, sweetening compositions are produced by spray drying solutions of an edible bulking agent and a di-peptide sweetening compound.
Readily soluble, sweetening compositions are produced by spray drying solutions of an edible bulking agent and a di-peptide sweetening compound.
Description
~039567 This invention relates to a readily soluble sweetening compositlon containing an edible bulking agent and a dipeptide sweetening agent. More particularly, it relates to a speci~ic method of spray drying a low bulk density sweetening composition which results in a composition having extremely rapid solubility in water and a bulk density and caloric value per unit of volume considerably less than that of sucrose.
Previous attempts to produce artificial sweeteners have involved the use of saccharins and/or cyclamates. Chief among these have been attempts to produce table sweeteners which have the appearance, behavior-in-use and sweetening intensity of sucrose per unit volume such as is taught in United States Patent No.
3,320,074 issued May 16, 1967. Specifically, this Patent teaches a method of spray drying an aqueous solution of saccharin and/or cyclamate whereas the solution is aerated with a non-reactive, non-inflammable gas, the amount of aeration gas defining the bulk -density of the final product.
Similarly~ United States Patent No. 3,170,801 issued February 23, 1965 teaches a method of deriving a table sweetener having the desirable organoleptic properties of sucrose by spray drying a solution of an artificial sweetener such as saccharin or cyclamate, a water dispersible edible protein whipping agent and a slurry of lactose into which a soluble gas has been intro-duced prior to drying. Problems have arisen with the use oP
these compounds, however, since the saccharins leaves a somewhat bitter aftertaste in the mouth and the cyclamates are now excluded from commercial food products as hazardous to human health.
It has recently been found that certain dipeptide com-pounds possess an intense sweetness level. Examples of these compounds are set forth in United States Patent Nos. 3,475,403 and 3,492,131. Most suitable among these compounds are the lower alkyl esters of aspartylphenylalanine wherein the stereochemical configuration is L-L, DL-DL, DL-L or L-DL. Illustrative o~`the ~3~567 lower alkyl esters are methyl, ethyl, propyl, butyl, pentylg hexyl, heptyl and the branched chain groups isometric therewlth, with the methyl ester being the most preferred embodiment.
These dipeptide materials would appear to have great commercial applications as sweetening agents since they range up to 200 times the sweetness level of sucrose, have no discernible unpleasant aftertaste and can be produced from naturally occurring amino aclds. Problems have arisen, however, with the use of these compounds in that their rate of solution into water is markedly slower than sucrose and that the compounds tend to decom-pose, losing substantially all their sweetness upon heating at temperatures above about 80C.
It has now been found that the rate of solution of dipeptide sweetening compounds can be significantly increased by spray-drying an aqueous solution of an edible bulking agent and the dipeptide sweetening compound. The specific method utilized in this invention produces a sweetening composition havin~ at least as rapid a rate of solubility as a freeze-dried sample on contact with water and as a result eliminates the tendency of spray dried sweeteners to float as a cohesive mass on the surface of beverages. In addition, utilization of this spray-drying method excludes the need for aerating the sweetener solution with gases that may affect the taste of the resultant product as well as cause extensive foaming problems when added to aqueous systems such as beverages. It has also been found that, surprisingly, these aqueous solutions may be spray-dried at conditions of elevated temperatures specifically, at temperatures as high as ~rom 300F. to 500F., without significant adverse effects on the sweetening level of the dipeptide compounds.
According to the invention there is provided a sweeten-ing composition containing a finely divided and dispersed lower alkyl ester of aspartylphenylalanlne having a sweetening power similar to sucrose in a matrix comprising a spray-dried spherical -- ... :
~03951 ;7 light reflec~ve powder of low bulk denslty in relation to that of sucrose between about 0.12 and 0.14 and a rapid solubility in water, said powder having as its ma~or bulking agent a dextrinose enzymatic starch hydrolysate having a dextrose equivalency o~
about 4 to 20 and an irregular distribution of other low sac-charides which are preponderently hexameric and heptameric.
There is also provided a method for producing a rapidly soluble sweetening composition comprising the steps of forming an aqueous solution of an edible bulking agent and L-aspartyl-L-phenylalanine meth~l ester, said bulking agent being selectedfrom the group consisting of organic acids, hydrolyzed starch materials and sugars, said aqueous solution containing less than one part L-aspartyl-L-phenylalanine methyl ester per part of bulk-ing agent and spray drying the solution at a feed concentration of not less than about 50% solids in a spray dryer apparatus having an inlet air temperature of about 350~. to about 500F.
The solid edible bulking agents suitable for use in this invention may be any of the non-toxic substances or combination of substances heretofore employed by the prior art for this pur-pose including the organic acids such as citric, adipic, malictartaric, fumaric acids and the hydrolyzed starch materials such as dextrins and sugars. Especially suitable among these solid bulking agents are the dextrins, particularly the low dextrose equivalent (D.E.) dextrins of the class commonly known as corn syrup solids. These materials are pre~erred not only because they are low in caloric content and non-hygroscopic but also due to the fact that they have a low bulk density which results in a caloric value per unit of bulk that is less than sucrose though its sweetness is equivalent to sucrose, the resulting composi-tion has the crystalline appearance of table sugar and dissolvesrapidly in cold water.
According to one embodiment of this invention, a table sugar substitute having the appearance of crystalline sucrose may . .. . ' ~039567 be prepared by forming a uniform aqueous solution o~ a corn syrup dextrin material and a dipeptide sweetening agent and spray-drying this solution in a manner so as to yield an expanded product which may then, if necessary, be ground to size. The method of spray-drying of this invention concerns introducing an aqueous solution of the bulking agent and dipeptide swee-tener preferably maintained at a temperature of about 150F. to 160F.
for reasons of complete dissolution of the dipeptide, into the spray dryer. Prior to feeding the solution into the spray drier, the solution is preferably pumped from the container through an in-line strainer to the dryer feed pump which is equipped with a homogenizing head. Thus, when the strained feed solution is sprayed into the dryer itself, the particle size Or undissolved sweetener particles is further reduced. Accordingly, the feed solution is pumped and sprayed downward and co-current with the drying air within the spray dryer. In order that the desired density of the spray-dried sweetening composition be derived, the feed concentration and inlet alr temperatures are critical. For the purposes of producing the table sweetener of this invention which preferably has a density of from about .12 to about .14, a feed concentration of usually not appreciably below about 50%
and preferably about 60% on an "as is" solids basis at an inlet air temperature of about 450F. is preferred. However, inlet air temperatures of as low as 300F. and as high as 500~. may be used, the densities varying inversely with temperatures and con-centration. Inlet temperature of below about 350~., however, will yield-end products having densities ranging from abo~t 0.2 to about 0.3. The air outlets, although not critical to this inven-tion, are preferably maintained at from about 225F. to about 270Fo~ an air outlet of 230F. at a flow of 2400 cpm being most preferred. Thus, where, for example, a density of 0.35 to 0.25 is desired, the feed concentration is accordingly ad~usted to about 30% to 40% with an air inlet temperature of about 300F.
--4-- ~ -- . .
~39567 Modification of thls procedure for variance of densities derived s~ould be obvious to those skilled in the art.
Since dextrins require great care in drying due to both fire and explosion hazards, this specific method of spray drylng results in operation at about half the lower explosion limit.
Thus, it should be obvious to those skilled in the art that further provisions for explosion supression devices and a high venting capability in the equipment, i.e., 1 ft.2 venting area per 25-40 cu. ~t., may permit use of higher capacities through use of higher feed concentration and higher inlet air temperatures with relative safety. Such conditions, in turn, would tend to produce a product of even lower denslty.
This method of spray drying was found unexpectedly to produce a sweetening composition having at least as great a rate of solubility than even a freeze-dried sample. Freeze-drying is ordinarily associated with producing dried compositions of such low density as to make them rapidly soluble but, unfortunately, is an extremely expensive process. This invention affords a method of drying whereat the resultant composition is not only at least as fast dissolving as a freeze-dried sample, but is also less expensive to produce.
The dextrin material used for the production of these sugar substitutes must dissolve easily in water to produce a clear solution and must be non-hygroscopic. In this regard, the D.E. (dextrose equivalent) of the dextrin material has been found to be a critical parameter. The dextrin material must have a suf-ficiently low mo--lecular weight to be easily soluble in water and to produce a clear solution so that the final product will have the essential reflecting surfaces in order to give the appearance of a crystalline product. On the other hand, the molecular weight of the dextrin material must be high enough so that hygroscoplcity is avoided.
Accordingly, it has been determined that for the produc-.. .. . .
. ~ - .
16~39567 tion of table sugar substitutes, the dextrin material should have a D.E. in the range o~ about 4 to 20 and preferably in the range of about 5 to 10. Additionally, it ~as been found that the best results are obtained if the dextrin material contains an irregular distribution of the other lower (one to eight saccharide units) saccharides with a preponderance of the hexamer and heptamer.
Such corn syrup dextrins have been produced by means of enzymatic hydrolysis of starch and are typified by the products available from CPC under the name Mor-Rex.
Consequently, the aforementioned specific method of spray-drying when applied to an aqueous solution comprised of a dextrin preferably a low D.E. dextrin such as Mor-Rex and a lower alkyl ester of aspartylphenylalanine, preferably L-aspartyl-L-phenylalanine methyl ester is the preferred embodiment of this lnvention. The spray-dried product of this invention consists of fairly uniform small, white spheres which reflect light in a way which suggests crystallinity are readily and completely soluble in water and produce clear aqueous-based solutions.
The processes of this invention are further illustrated 0 but not limited by the ~ollowing examples:
Three grams of citric acid and one gram of L-aspartyl-L-phenylalanine methyl ester are dissolved in 50 ml. o~ water with stirring. The resulting solution is spread on a stainless steel tray (2.1 sq. ft.) and allowed to dry at ambient conditions for about two days. The dry material was then scraped from the tray and ground with a mortar and pestle. One-half gram samples of this ground material were added, with stirring, to beakers containing 200 ml. of water at 40F. The material completely dis-solved in an average time of about 55 seconds yielding solutionswhich were sweet with a slight acid taste.
A solution was prepared containing 800 grams of water -r~D~
... .....
1C1~395~i7 (80F.), 241 grams of 5 D.E. Mor-Rex and 5.95 grams of L-aspartyl L-phenylalanine methyl ester. This solution was placed in a tray at a 1.5 inch thickness and freeze dried in a Stokes Freeze Drier~
- for 48 hours. The material was then ground to a fine powder using a Waring Blende ~at a high speed.
A solution was prepared according to the method of Example 2 and this solution was drum dried at a temperature of 130C. on a drier operating at 25 lbs./sq.in and 6.25 rpms.
A solution containing 384.05 grams o~ water, 241 grams of 5 D.E. Mor-Rex~and 5.95 grams of L-aspartyl-L-phenylalanine methyl ester was prepared. This solution was then spray dried in a Niro Spray Dryer~at an air pressure of 5.2 kg/sq. cm., an air inlet temperature of 160C. (320F.), an air outlet temperature of 75C. (167F.) and a rate of solution flow of 15 co/min.
Equal weight samples of the sweetening compositions of Examples ?, 3 and 4 were dissolved in coffee samples and were organoleptically determined.to have a substantially equivalent sweetness level. This sweetness level is not found to signifi-cantly differ from control coffee samples containing an equal amount of the untreated dlpeptide material, thus indicating the absence of any degradation of the ~ipeptide material during the drying operations. The rate of solubility, however, is appreci-ably and substant~ally improved.
The solubility rate of the powders from Examples 2, 3 and 4 was evaluated by recording the times required for complete solution of 1.5 gra~ samples of these powders (containing about o.o36 grams of sweetener) into 170 ml. of water at a temperature of 40F., with stirring. The results are summarized in the table below:
40F (time in seconds) Example 2 62 Example 3 40 Example 4 60 ~k -rR~ y~ _7_ 1~39567 As is evident rrom the above data, the specific method of spray-drying utilized resulted in a product having an equiva lent rate of solubility as the freeze-drled sample.
When 0.036 gram samples of L-aspartyl-L-phenylalanine methyl ester are sought to be di~solved in 170 ml. of water at 40F., with s~irring, average times for complete solution run about 30 minutes.
Additional tests have shown that varying the level of dipeptide in the sweetening compositions up to the level of about one part dipeptide per part of bulking agent, does not have any appreciable or predictable effect on the rate of solution.
It has also been found that the elevated temperatures, in excess of 100C~g which are employed during the spray drying operation of this invention does not effect the sweetness of the final product.
The bulk density of the final sweetening composition can be controlled by varying the solids concentration of the solu-tion prior to spray drying. The bulk density may also be con-trolled by changing the method of drying, by varying the rate of drying, or by varying the conditions of pressure under which the solution is dried. Bulk densities ranging as low as about 0.04g/-cc can be obtained Oy the process of the instant invention.
The addition of a small amount of an anti-caking agent such as trlcalcium phosphate may also be used to adjust the bulk density of the final product.
Thus, by exercising proper control over the process, it is possible to produce a final product which has substantially the same bul~ density of granulated sucrose or a product which has a much lower bulk density than granulated sucrose, but which, by ad~
~usting the level of dipeptide sweetening compound, has on a volume basis the same level of sweetness as sucrose, but a far less caloric value. More importantly, the resulting spray-dried product has a substantially greater rate of solubility and greater .. . . : . .
. :~ - : -.
absolute solubllity in water.
A sweetening composition which has on a volume basis the same sweetening power of sucrose is prepared by spray-drying a 50% solids solution containing 96.5%, 10 D.E. Mor-Rex and 3.5% L-aspartyl-L-phenylalanine. The drier was equipped with a single l/lTC Whirl~et nozzle and was operating with a spray pressure of 500 to 700 psig., an inlet air temperature of 400F., an air flow of 2800 cu. ft./min., an air outlet temperature of 245F. and a feed temperature of 155F. The spray-dried powder was screened through a 16 U.S. mesh screen and blended with 0.1% by weight of tricalcium phosphate. The resultant product has a bulk density of 0.14 g/cc, has a crystalline appearance, has, on a volume basis, the same level of sweetness as granulated table sugar and dissolves rapidly in 40F. water.
The density obtained above can be modified, particularly increased, by employing suitable agglomeration techniques such as applying moisture to a falling curtain of material as disclosed in Patents to Sienkiewicz, et al. or in belt agglomeraters or the like.
~ ~R~
_g _ - .
. . . - , . .
.. ~ - . .. . .
Previous attempts to produce artificial sweeteners have involved the use of saccharins and/or cyclamates. Chief among these have been attempts to produce table sweeteners which have the appearance, behavior-in-use and sweetening intensity of sucrose per unit volume such as is taught in United States Patent No.
3,320,074 issued May 16, 1967. Specifically, this Patent teaches a method of spray drying an aqueous solution of saccharin and/or cyclamate whereas the solution is aerated with a non-reactive, non-inflammable gas, the amount of aeration gas defining the bulk -density of the final product.
Similarly~ United States Patent No. 3,170,801 issued February 23, 1965 teaches a method of deriving a table sweetener having the desirable organoleptic properties of sucrose by spray drying a solution of an artificial sweetener such as saccharin or cyclamate, a water dispersible edible protein whipping agent and a slurry of lactose into which a soluble gas has been intro-duced prior to drying. Problems have arisen with the use oP
these compounds, however, since the saccharins leaves a somewhat bitter aftertaste in the mouth and the cyclamates are now excluded from commercial food products as hazardous to human health.
It has recently been found that certain dipeptide com-pounds possess an intense sweetness level. Examples of these compounds are set forth in United States Patent Nos. 3,475,403 and 3,492,131. Most suitable among these compounds are the lower alkyl esters of aspartylphenylalanine wherein the stereochemical configuration is L-L, DL-DL, DL-L or L-DL. Illustrative o~`the ~3~567 lower alkyl esters are methyl, ethyl, propyl, butyl, pentylg hexyl, heptyl and the branched chain groups isometric therewlth, with the methyl ester being the most preferred embodiment.
These dipeptide materials would appear to have great commercial applications as sweetening agents since they range up to 200 times the sweetness level of sucrose, have no discernible unpleasant aftertaste and can be produced from naturally occurring amino aclds. Problems have arisen, however, with the use of these compounds in that their rate of solution into water is markedly slower than sucrose and that the compounds tend to decom-pose, losing substantially all their sweetness upon heating at temperatures above about 80C.
It has now been found that the rate of solution of dipeptide sweetening compounds can be significantly increased by spray-drying an aqueous solution of an edible bulking agent and the dipeptide sweetening compound. The specific method utilized in this invention produces a sweetening composition havin~ at least as rapid a rate of solubility as a freeze-dried sample on contact with water and as a result eliminates the tendency of spray dried sweeteners to float as a cohesive mass on the surface of beverages. In addition, utilization of this spray-drying method excludes the need for aerating the sweetener solution with gases that may affect the taste of the resultant product as well as cause extensive foaming problems when added to aqueous systems such as beverages. It has also been found that, surprisingly, these aqueous solutions may be spray-dried at conditions of elevated temperatures specifically, at temperatures as high as ~rom 300F. to 500F., without significant adverse effects on the sweetening level of the dipeptide compounds.
According to the invention there is provided a sweeten-ing composition containing a finely divided and dispersed lower alkyl ester of aspartylphenylalanlne having a sweetening power similar to sucrose in a matrix comprising a spray-dried spherical -- ... :
~03951 ;7 light reflec~ve powder of low bulk denslty in relation to that of sucrose between about 0.12 and 0.14 and a rapid solubility in water, said powder having as its ma~or bulking agent a dextrinose enzymatic starch hydrolysate having a dextrose equivalency o~
about 4 to 20 and an irregular distribution of other low sac-charides which are preponderently hexameric and heptameric.
There is also provided a method for producing a rapidly soluble sweetening composition comprising the steps of forming an aqueous solution of an edible bulking agent and L-aspartyl-L-phenylalanine meth~l ester, said bulking agent being selectedfrom the group consisting of organic acids, hydrolyzed starch materials and sugars, said aqueous solution containing less than one part L-aspartyl-L-phenylalanine methyl ester per part of bulk-ing agent and spray drying the solution at a feed concentration of not less than about 50% solids in a spray dryer apparatus having an inlet air temperature of about 350~. to about 500F.
The solid edible bulking agents suitable for use in this invention may be any of the non-toxic substances or combination of substances heretofore employed by the prior art for this pur-pose including the organic acids such as citric, adipic, malictartaric, fumaric acids and the hydrolyzed starch materials such as dextrins and sugars. Especially suitable among these solid bulking agents are the dextrins, particularly the low dextrose equivalent (D.E.) dextrins of the class commonly known as corn syrup solids. These materials are pre~erred not only because they are low in caloric content and non-hygroscopic but also due to the fact that they have a low bulk density which results in a caloric value per unit of bulk that is less than sucrose though its sweetness is equivalent to sucrose, the resulting composi-tion has the crystalline appearance of table sugar and dissolvesrapidly in cold water.
According to one embodiment of this invention, a table sugar substitute having the appearance of crystalline sucrose may . .. . ' ~039567 be prepared by forming a uniform aqueous solution o~ a corn syrup dextrin material and a dipeptide sweetening agent and spray-drying this solution in a manner so as to yield an expanded product which may then, if necessary, be ground to size. The method of spray-drying of this invention concerns introducing an aqueous solution of the bulking agent and dipeptide swee-tener preferably maintained at a temperature of about 150F. to 160F.
for reasons of complete dissolution of the dipeptide, into the spray dryer. Prior to feeding the solution into the spray drier, the solution is preferably pumped from the container through an in-line strainer to the dryer feed pump which is equipped with a homogenizing head. Thus, when the strained feed solution is sprayed into the dryer itself, the particle size Or undissolved sweetener particles is further reduced. Accordingly, the feed solution is pumped and sprayed downward and co-current with the drying air within the spray dryer. In order that the desired density of the spray-dried sweetening composition be derived, the feed concentration and inlet alr temperatures are critical. For the purposes of producing the table sweetener of this invention which preferably has a density of from about .12 to about .14, a feed concentration of usually not appreciably below about 50%
and preferably about 60% on an "as is" solids basis at an inlet air temperature of about 450F. is preferred. However, inlet air temperatures of as low as 300F. and as high as 500~. may be used, the densities varying inversely with temperatures and con-centration. Inlet temperature of below about 350~., however, will yield-end products having densities ranging from abo~t 0.2 to about 0.3. The air outlets, although not critical to this inven-tion, are preferably maintained at from about 225F. to about 270Fo~ an air outlet of 230F. at a flow of 2400 cpm being most preferred. Thus, where, for example, a density of 0.35 to 0.25 is desired, the feed concentration is accordingly ad~usted to about 30% to 40% with an air inlet temperature of about 300F.
--4-- ~ -- . .
~39567 Modification of thls procedure for variance of densities derived s~ould be obvious to those skilled in the art.
Since dextrins require great care in drying due to both fire and explosion hazards, this specific method of spray drylng results in operation at about half the lower explosion limit.
Thus, it should be obvious to those skilled in the art that further provisions for explosion supression devices and a high venting capability in the equipment, i.e., 1 ft.2 venting area per 25-40 cu. ~t., may permit use of higher capacities through use of higher feed concentration and higher inlet air temperatures with relative safety. Such conditions, in turn, would tend to produce a product of even lower denslty.
This method of spray drying was found unexpectedly to produce a sweetening composition having at least as great a rate of solubility than even a freeze-dried sample. Freeze-drying is ordinarily associated with producing dried compositions of such low density as to make them rapidly soluble but, unfortunately, is an extremely expensive process. This invention affords a method of drying whereat the resultant composition is not only at least as fast dissolving as a freeze-dried sample, but is also less expensive to produce.
The dextrin material used for the production of these sugar substitutes must dissolve easily in water to produce a clear solution and must be non-hygroscopic. In this regard, the D.E. (dextrose equivalent) of the dextrin material has been found to be a critical parameter. The dextrin material must have a suf-ficiently low mo--lecular weight to be easily soluble in water and to produce a clear solution so that the final product will have the essential reflecting surfaces in order to give the appearance of a crystalline product. On the other hand, the molecular weight of the dextrin material must be high enough so that hygroscoplcity is avoided.
Accordingly, it has been determined that for the produc-.. .. . .
. ~ - .
16~39567 tion of table sugar substitutes, the dextrin material should have a D.E. in the range o~ about 4 to 20 and preferably in the range of about 5 to 10. Additionally, it ~as been found that the best results are obtained if the dextrin material contains an irregular distribution of the other lower (one to eight saccharide units) saccharides with a preponderance of the hexamer and heptamer.
Such corn syrup dextrins have been produced by means of enzymatic hydrolysis of starch and are typified by the products available from CPC under the name Mor-Rex.
Consequently, the aforementioned specific method of spray-drying when applied to an aqueous solution comprised of a dextrin preferably a low D.E. dextrin such as Mor-Rex and a lower alkyl ester of aspartylphenylalanine, preferably L-aspartyl-L-phenylalanine methyl ester is the preferred embodiment of this lnvention. The spray-dried product of this invention consists of fairly uniform small, white spheres which reflect light in a way which suggests crystallinity are readily and completely soluble in water and produce clear aqueous-based solutions.
The processes of this invention are further illustrated 0 but not limited by the ~ollowing examples:
Three grams of citric acid and one gram of L-aspartyl-L-phenylalanine methyl ester are dissolved in 50 ml. o~ water with stirring. The resulting solution is spread on a stainless steel tray (2.1 sq. ft.) and allowed to dry at ambient conditions for about two days. The dry material was then scraped from the tray and ground with a mortar and pestle. One-half gram samples of this ground material were added, with stirring, to beakers containing 200 ml. of water at 40F. The material completely dis-solved in an average time of about 55 seconds yielding solutionswhich were sweet with a slight acid taste.
A solution was prepared containing 800 grams of water -r~D~
... .....
1C1~395~i7 (80F.), 241 grams of 5 D.E. Mor-Rex and 5.95 grams of L-aspartyl L-phenylalanine methyl ester. This solution was placed in a tray at a 1.5 inch thickness and freeze dried in a Stokes Freeze Drier~
- for 48 hours. The material was then ground to a fine powder using a Waring Blende ~at a high speed.
A solution was prepared according to the method of Example 2 and this solution was drum dried at a temperature of 130C. on a drier operating at 25 lbs./sq.in and 6.25 rpms.
A solution containing 384.05 grams o~ water, 241 grams of 5 D.E. Mor-Rex~and 5.95 grams of L-aspartyl-L-phenylalanine methyl ester was prepared. This solution was then spray dried in a Niro Spray Dryer~at an air pressure of 5.2 kg/sq. cm., an air inlet temperature of 160C. (320F.), an air outlet temperature of 75C. (167F.) and a rate of solution flow of 15 co/min.
Equal weight samples of the sweetening compositions of Examples ?, 3 and 4 were dissolved in coffee samples and were organoleptically determined.to have a substantially equivalent sweetness level. This sweetness level is not found to signifi-cantly differ from control coffee samples containing an equal amount of the untreated dlpeptide material, thus indicating the absence of any degradation of the ~ipeptide material during the drying operations. The rate of solubility, however, is appreci-ably and substant~ally improved.
The solubility rate of the powders from Examples 2, 3 and 4 was evaluated by recording the times required for complete solution of 1.5 gra~ samples of these powders (containing about o.o36 grams of sweetener) into 170 ml. of water at a temperature of 40F., with stirring. The results are summarized in the table below:
40F (time in seconds) Example 2 62 Example 3 40 Example 4 60 ~k -rR~ y~ _7_ 1~39567 As is evident rrom the above data, the specific method of spray-drying utilized resulted in a product having an equiva lent rate of solubility as the freeze-drled sample.
When 0.036 gram samples of L-aspartyl-L-phenylalanine methyl ester are sought to be di~solved in 170 ml. of water at 40F., with s~irring, average times for complete solution run about 30 minutes.
Additional tests have shown that varying the level of dipeptide in the sweetening compositions up to the level of about one part dipeptide per part of bulking agent, does not have any appreciable or predictable effect on the rate of solution.
It has also been found that the elevated temperatures, in excess of 100C~g which are employed during the spray drying operation of this invention does not effect the sweetness of the final product.
The bulk density of the final sweetening composition can be controlled by varying the solids concentration of the solu-tion prior to spray drying. The bulk density may also be con-trolled by changing the method of drying, by varying the rate of drying, or by varying the conditions of pressure under which the solution is dried. Bulk densities ranging as low as about 0.04g/-cc can be obtained Oy the process of the instant invention.
The addition of a small amount of an anti-caking agent such as trlcalcium phosphate may also be used to adjust the bulk density of the final product.
Thus, by exercising proper control over the process, it is possible to produce a final product which has substantially the same bul~ density of granulated sucrose or a product which has a much lower bulk density than granulated sucrose, but which, by ad~
~usting the level of dipeptide sweetening compound, has on a volume basis the same level of sweetness as sucrose, but a far less caloric value. More importantly, the resulting spray-dried product has a substantially greater rate of solubility and greater .. . . : . .
. :~ - : -.
absolute solubllity in water.
A sweetening composition which has on a volume basis the same sweetening power of sucrose is prepared by spray-drying a 50% solids solution containing 96.5%, 10 D.E. Mor-Rex and 3.5% L-aspartyl-L-phenylalanine. The drier was equipped with a single l/lTC Whirl~et nozzle and was operating with a spray pressure of 500 to 700 psig., an inlet air temperature of 400F., an air flow of 2800 cu. ft./min., an air outlet temperature of 245F. and a feed temperature of 155F. The spray-dried powder was screened through a 16 U.S. mesh screen and blended with 0.1% by weight of tricalcium phosphate. The resultant product has a bulk density of 0.14 g/cc, has a crystalline appearance, has, on a volume basis, the same level of sweetness as granulated table sugar and dissolves rapidly in 40F. water.
The density obtained above can be modified, particularly increased, by employing suitable agglomeration techniques such as applying moisture to a falling curtain of material as disclosed in Patents to Sienkiewicz, et al. or in belt agglomeraters or the like.
~ ~R~
_g _ - .
. . . - , . .
.. ~ - . .. . .
Claims (8)
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A method for producing a rapidly soluble sweetening composition having a bulk density in relation to that of sucrose between about 0.12 and 0.14 and containing a finely divided and dispersed lower alkyl ester of aspartylphenylalamine having a sweetening power similar to sucrose in a matrix comprising a spray-dried spherical light reflective powder of low bulk density in relation to that of sucrose between about 0.12 and 0.14 and a rapid solubility in water, said powder having as its major bulk-ing agent a dextrinose enzymatic starch hydrolysate having a dextrose equivalency of about 4 to 20 and an irregular distri-bution of other low saccharides which are preponderently hexa-meric and heptameric, comprising the steps of forming an aqueous solution containing less than one part of the said lower alkyl ester per part of said powder and spray drying the solution at a feed concentration of not less than about 50% solids in a spray dryer apparatus having an inlet air temperature of about 350° F. to about 500° F.
2. A method for producing a rapidly soluble sweetening composition having a bulk density in relation to that of sucrose between about 0.12 and 0.14 and containing a finely divided and dispersed lower alkyl ester of aspartylphenylalamine having a sweetening power similar to sucrose in a matrix comprising a spray-dried spherical light reflective powder of low bulk density in relation to that of sucrose between about 0.12 and 0.14 and a rapid solubility in water, said powder having as its major bulking agent a dextrinose enzymatic starch hydrolysate having a dextrose equivalency of about 4 to 20 and an irregular distribut-ion of other low saccharides which are preponderently hexameric and heptameric, comprising the steps of forming an aqueous solu-tion containing less than one part of the said lower alkyl ester per part of said powder and spray drying the solution at a feed concentration of about 60% solids in a spray dryer apparatus having an inlet air temperature of about 450° F.
3. A method according to claim 2, wherein the spray dryer apparatus has an outlet air temperature of from about 225°F.
to about 270°F.
to about 270°F.
4. A method according to claim 3, wherein the outlet air temperature is about 230°F.
5. A method according to claim 4, wherein the aqueous solution is maintained at a temperature of about 150°F. to about 160°F. while being introduced into the spray dryer.
6. A method according to claim 1, or 2, wherein the solution is pumped through an in-line strainer to the spray dryer feed pump equipped with a homogenizing head.
7. A method according to claim 1, or 2, wherein the aqueous solution is pumped and sprayed downward and co-current with the drying air into the spray dryer.
8. A rapidly soluble sweetening composition having a bulk density in relation to sucrose between about 0.12 and 0.14 and containing a finely divided and dispersed lower alkyl ester of aspartylphenylalanine having a sweetening power similar to sucrose in a matrix comprising a spray-dried spherical light reflective powder of low bulk density in relation to that of sucrose between about 0.12 and 0.14 and a rapid solubility in water, said powder having as its major bulking agent a dextrinose enzymatic starch hydrolysate having a dextrose equivalency of about 4 to 20 and an irregular distribution of other low sacchar-ides which are preponderently hexameric and heptameric.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US05/387,848 US4001456A (en) | 1970-07-16 | 1973-08-13 | Low calorie sweetening composition and method for making same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1039567A true CA1039567A (en) | 1978-10-03 |
Family
ID=23531578
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA206,437A Expired CA1039567A (en) | 1973-08-13 | 1974-08-07 | Low calorie sweetening composition and method for marking same |
Country Status (1)
| Country | Link |
|---|---|
| CA (1) | CA1039567A (en) |
-
1974
- 1974-08-07 CA CA206,437A patent/CA1039567A/en not_active Expired
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