Europaisches P a t e n t a m t © European Patent Office © Publication number: Office europeen des brevets 0 000 077 A1 E U R O P E A N PATENT A P P L I C A T I O N © © Application number: 78200015.2 0 Int. CI.2: A 23 L 2 / 3 8 © Date of filing: 01.06.78 © Priority: 03.06.77 US 803337 © Date of publication of aoplication: 20.12.71 Bulletin 78/1 © Designated Contracting States: BE CH6EFRGBLUNI.se © Applicant: THE PROCTER &GAMBLE COMPANY, 301 East Sixth Street, Cincinnati, Ohio (US) © Inventor: McCarty, Charles Bruce, 2921 WerkRoad, Cincinnati, OH (US) © Inventor: Sampson, Ronald Lee, 1580 Tremont Lane, Cincinnati, OH 45224 (US) © Representative: Munro, Hamish David et al, PROCTER & GAMBLE EUROPEAN TECHNICAL CENTER Temselaan 100, 1820 - Strombeek-Bever (BE) © Dry-carbonated beverage mixes and method for the preparation of beverages therewith. A substantially dry fructose-seetened dietetic, carbonated beverage mix comprising a crystalline fructose sweetener, a flavorant, an acidulant and an amount effective to carbonate a beverage of carbon dioxide-loaded zeolitic molecular sieve material. At the point of consumption, when a beverage-making liquid is brought into contact with the mix, a fructose-sweetened, dietetic, carbonated beverage is provided. The instant dry beverage mix of the present invention provides a higher level of sweetness in a dietetic carbonated beverage than other liquid beverage systems sweetened with predissolved fructose or other natural sugars whether solid or liquid on a calorie-for-calorie basis. The dry instant beverage mix herein provides a faster rate of carbonation of the beverage prepared therefrom than is provided by similar instant dry beverage mixed in which sucrose is the primary sweetener. This mix for it are dietetic relates free in the .sitions relates carbonated to n a t u r a l l y sweetened The p r e p a r a t i o n of p o t a b l e sweetened art. dry beverage Depending included dry beverage beverages, by d i s s o l u t i o n upon the in such mixes, beverage More p a r t i c u l a r l y , beverages. sweeteners. beverages, carbonated to a dry of a r t i f i c a l carbonated ficially invention mixes particularly an a r t i - of a n a t u r a l o r mix in water nature of the beverages which has been d e s c r i b e d various prepared compo- there from may be c h a r a c t e r i z e d The d i e t e t i c by c a l o r i c carbonated beverages heretofore been made with sweeteners appeared down but non-dietetic considered ill-advised taken in drink. been widely include like is persons, sugar of Kennedy et al. a non-sugar et al. or that a suitable as molecular G. Singh do n o t , sweetener sieves and T. however, a suitably in J. in mention an a l l - f r u c t o s e - s w e e t e n e d or not e.g., Patent low-calorie dry m i x . mix Kennedy mix com- However, sweetened the with aspartame. suitable system 3,930,053 December discuss or 1975), carrier. a dry-mix U.S. are, Shires J. beverage primarily agent, Kennedy, sweetened, 21, April among a number of disclosed, There beverage and P h i l i p sugar dry mix is sweetening dipeptide have beverage. carbonated a crystalline low-calorie Fructose'is Japikse, low-calorie a dry been who should carbonated filed or low c a l o r i e sweeteners- obese, Kennedy 570,332, have purpose. carbonated J. Timothy content but who do not want of a l o w - c a l o r i e disclose with diet Illustrative from 7-30% of tion their sweetened prising sugars, the e.g., the forbidden sweetened this for calories caloric and artificial artificially composition al. from in Patent Application (U.S. et excessive the the and u t i l i z e d a number of however, hand, approaches a suitably certain Most n o t a b l y , accepted other a high Numerous to p r o v i d e an a t t e m p t soft others. Artificial the On the contain have to keep to the w e i g h t - c o n s c i o u s certain for in order sweetness. beverages unattractive from such mixes sweeteners. to be n e c e s s a r y carbonated as dietetic or n o n - d i e t e t i c . prepared artificial effective provide content 30, dietetic beverage in comb.ina- to C. H. 1975. 'Japikse beverages could be made For maximum c o n v e n i e n c e devices of the beverage not mention worse, dry it herein, rate fructose-sweetened insufficient of fructose passage of dietetic unstable time. of c a r b o n a t i o n the at rate be r a p i d . Japikse may have, of the to t h e i r fructose sweetness is that of c a r b o n a t i o n carbonation Although carbonation which fructose mix a c c o r d i n g sieve molecular desirable made t h e r e w i t h any e f f e c t on the beverage is in use of the for beverage invention et al do better made with or a . and a CO2-loaded device. is the sweetest carbonated dietetic in l i q u i d natural beverage levels, systems for sugar, a liquid is hampered the sweetest and d i m i n i s h e s by form with the OBJECTS OF THE INVENTION It tive has for sweetness carbonated dry been sweetness the in soft sweetened dietetic It is, therefore, beverage. is It a method for the come c e r t a i n fructose the which is a dry carbonation It fructose the beverage a further is is a method of the present a liquid maximizes device provision of the the provide rate the loss invention power of the p r e s e n t to fructose with invention provide in t o a suitable of c a r b o n a t i o n of the dietetic the of system. of t h e or m a x i m i z e d . object over- a particular system. which maximizes in a p a r t i c u l a r is much of present sweetening it object, to overcome mix in c o m b i n a t i o n increased another latter of with art. beverage object whereby to which beverages to dietetic of a sweet invention dietetic in invention combination mix in the the object beverage beverage with of t h e present for prior another dietetic It provide in the liquid. to a r t i f i c i a l l y of the dry b e v e r a g e invention present is It particular of object inven- fructose particularly an o b j e c t fructose connection sweetness a method of or f l e e t i n g a primary an o b j e c t use the beverages. device problems In of also via beverage an a l t e r n a t i v e a fructose-sweetened, carbonated final is It effec- can provide of t h e p r e s e n t systems, carbonated carbonation provide liquid provide a suitable object carbonated diminished drinks. invention to present provide to fructose mix and method beverage developed carbonated that a dietetic in c o n t r a s t tion, found present invention sweetening carbonated to power o f beverage system. a SUMMARY OF THE INVENTION The p r e s e n t a surprisingly carbonated dietetic, fructose crystalline The c a r b o n a t i o n at the into point contact device with sieve preferred instant fructose as a mix which, carbonation rapidly at beverage molecular is sweetener device the point sweetened sieve yields with and an device. the b e v e r a g e brought A C02-loaded liquid. container a C02-loaded a beverage sucrose carbonation present mix is instant dry beverage of consumption with to c a r b o n a t e use of e s s e n t i a l l y in the when c a r b o n a t e d the is a device. the that at carbonation in a s e r v i n g carbonation is found the affixed a mix, mix o f t h e a flavorant when said a beverage-making disc carbonating low-calorie, beverage an i n s t a n t effective of consumption molecular It with that amount of an e s s e n t i a l l y sweetener, in c o m b i n a t i o n acidulant, dry, instant The dry an e f f e c t i v e comprises rapidly by a method of adding carbonated fructose-sweetened invention dietetic, to an i n s t a n t , liquid of c o n s u m p t i o n . point pure is p r o v i d e d beverage on the d i s c o v e r y based low-calorie, sweet, beverage-making is invention which than does crystalline mix h e r e i n molecular carbonates and c a r b o n a t e d device. pure provides sieve more a carbonated with a C02-loaded A beverage has only about 6 calories has an e f f e c t i v e prisingly 'enjoyment during of beverage tains of made in the level the the of ounce of is for but the words, but sweet, and c a l o r i c weight sur- consumer In o t h e r acceptably sugar invention present serving, sweetness periods. invention one-half ncn-dietetic fluid serving present about only per average with accordance con- content beverages. DESCRIPTION OF THE PREFERRED EMBODIMENTS with In a c c o r d a n c e low-calorie, dietetic, the rapidly fructose (2) sweetener, an i n s t a n t when an e f f e c t i v e into contact device made therefrom free of a r t i f i c i a l The dry mix is of essentially as used fructose" and a g g l o m e r a t e d herein flavor sugar made method liquid) tive of carrier, but perceptible of at the carrier. a liquid amount brought beverage an e f f e c t i v e t a m o u n t with dried other pure fructose powders, crystalline comprising flavorant, a crystalline the Such flavorant, flavor forming granules, a uniform carrier. levels dry-mixed acidulant are crystals an a c i d u l a n t , concentration sweetness. the sugar is sweetener fructose comprising crystals crystalline by the is powders. Preferably, dried a beverage liquid "essentially includes (4) sweeteners. fructose The term ingredients. beverage and to c a r b o n a t e made by dry mixing crystalline pure pure c r y s t a l l i n e The dry mix and the dry mix. the are effective dry, beverage mix an a c i d u l a n t (3) of a b e v e r a g e - m a k i n g amount with an e s s e n t i a l l y a flavorant, carbonation carbonated carbonating of the present invention is made from (1) the invention, present (or a t h i c k and a minor involved and'a preferably slurry Sucrose with is but effec- a preferred contributes no The uniform manner, vacuum-dried e.g., flavor crystals. fructose a preferred, stable, and dry 4% to the dry beverage mix. embodiment of the pure sugar from In o t h e r carrier about the of dry flavor fructose of 96% by weight Another the gives fructose crystals constitute from about mix. beverage is of The c r y s t a l which sucrose said dry flavor constitutes consti- crystals. from about 88% mix. beverage way to make the crystals dry c r y s t a l l i n e crystals dry dry mix com- sweetener the flavor dry dry beverage 40% by weight 20% to the words, about of 12% by weight substantially amount of the the flavor crystals in which the flavor about tutes to with a dry mix of e s s e n t i a l l y prises in a s u i t a b l e dehydrated an e f f e c t i v e sweetener A preferred line then to provide Admixing crystalline is slurry dry b e v e r a g e mix of the present invention is to make a slurry of all the dry beverage mix ingredients including an effective amount of essentially pure crystalline f r u c t o s e sweetener uniform nation and beverage of said course, other obvious to methods those in dry a detailed practice mix. of combining in beverage beverage discussion of the the uniform and a c i d u l a n t . dry ccmbiOf the ingredients art. are these a substantially and d r y i n g flavorants mixes a substantially flavorant sweetener, skilled or u n d e r s t a n d to p r o v i d e same Such a mix is fructose Various useful the co-drying well and a c i d u l a n t known in components present is the systems art. unnecessary invention. Thus, to will be In affixed is disc the at carbonation. instant in useful Liepa a preferred the 8, February the Hendrikus of Liepa of 0.001 dry serving the is and mix beverage container discharged promote carbonation. inch are making from the to devices by A l e x a n d e r in U. S. Patent No. Leon - 4,007,134, its in by r e f e r e n c e sieve provide carbonation disclosed are carbonation sieve is to about is contact the block dissolution or entirety, 3 inches. put into with of the its the following the molded b l o c k having introduced, and device a single material enclosed When water cup. suitable incorporated and J a p i k s e molecular about of molecular container a serving Japikse instant of C 0 2 - l o a d e d from a C02-loaded drawings. A preferred teachings of invention herein 1977, particularly bottom Examples present Cornelis and embodiment, a thickness Both the block a container, preferably serves dry mix and p r o v i d e a ice, into over mix and b l o c k , discharge e.g., and the CO2 to a g i t a t e beverage The f r u c t o s e found to c a r b o n a t e which are herein. of molecular whether sweetened the mix p a r t i c l e s the This beverage affixed find in to the the whether placed serving effectiveness in the sweetness serving calorie, the point level dietetic, essentially is liquid does and the of the of a crystalline on or below t h e before devices carbonation with carbonation not depend above the beverages as d i s c u s s e d addition the ice. added preferably since container, are carbonated rate. of container serving herein similar pure placed or dry beverage The p r e s e n t the the use of c a r b o n a t i o n the the-device that mix h e r e i n device the making facilitates the beverage carbonation found is device carbonation is made with beverage fructose of it otherwise when each sucrose sieve Furthermore, the dry with mixes beverage than more r a p i d l y sweetened CO2-loaded sweetened which are not consumer will not device mix p a r t i c l e s affected are by first container. invention fructose rapidly provides in a method of m a x i m i z i n g a fructose-sweetened, carbonating carbonated low beverage at of c o n s u m p t i o n . By adding calorie, d i e t e t i c , a beverage-making liquid to the instant dry, low rapidly carbonating carbonated beverage mix a surprisingly level high of used beverage as calories per sweetener fructose herein fluid means of ounce accounts is sweetness for The term provided. which has a beverage Of c o u r s e , serving. all substantially of the "dietetic" 6 or the less fructose calories in the. beverage. No a r t i f i c i a l the resulting beverage all consumers to 3 to about made beverage device a molded supra, of elongated is surface disc is a in contact and ice can also making l extending in at place with preferred be used as i molecular effective the the liquid. Chilled beverage-making both the q u a dietetic sweetened. Patent 4,007,134, No. having surface the or an o p p o s i t e an amount when b r o u g h t beverage cool device The cup. having liquids. i a plurality to a serving water carbonation of a b o u t a carbona- material to'carbonate yet comprising of bottom sieve period serving, a disc from one but substantially effectively of U.S. form of the channels held are in is embodiment by FIG.3 for serving 14-ounce method preferred block dioxide carbon a 6- to or used, sweet an a v e r a g e instant C02-loaded of For illustrated needed surprisingly for the by In a n o t h e r tion is enjoy. 27 m i n u t e s is sweetener tap water Carbonated and d the water beverage. For best ice and results, serving cup c o n t a i n i n g provide a specified the total An a n t i - f o a m i n g mix. beverage for dry beverage to 3,983,251 to A rapidly The P r o c t e r integral The illustrated the not is . September the of in U.S. Patent 28, 1976, of the the this dry additive assigned The a n t i f o a m a n t crystals to in dry a n t i f o a m disclosed Company.. limited e to t h e mix t o beverage m dissolvable and methods can be a n mix. dry b e v e r a g e invention following are further Examples EXAMPLE I . Flavor A 200 Crystals g batch constitute about sweetener) of flows; u added are can be i n c l u d e d agent flavor products but l Singh, & Gamble of part o compositions Gyanendra carbonated dry v water 6.7 of parts a low-calorie Preparation flavor crystals, by dry weight dry b e v e r a g e which (93.3 mix, when u s e d parts fructose was p r e p a r e d as of All liquid ingredients into were weighed a container. single the All added slowly uniform to of ingredients dry the liquid a natural derived plant. into was p o u r e d of temperature flavor licorice the stainless were crystals flavor acceptable screened formulation, flavor mono- enhancer slurry product at 20 hours. a U.S.#12 retained is drink, and v a c u u m - d r i e d through a until the liquid approximately were crystals GRAS sweet trays for in ounce The t h i c k steel 100°F about fluid then separately, blending Present a 10.6 ammonium g l y c y r r h i z i n a t e , from while ingredients 15 ppm in about weighed were was o b t a i n e d . mixture slurry a level at the a The d r i e d and screen, the #20 s c r e e n . on a U.S. EXAMPLE I I Several dietetic 93.3 carbonated is with in for a total ounce 3 of U.S. the The b e v e r a g e g of drink, mix were prepared flavor dry fructose of ice is Patent is 17.05 rapidly sieve 4,007,134, placed in by dry a d m i x i n g g of the carbonated. 1.15 disc of Example g of ice a serving like supra. the cup and cool mix p e r (3.55 cup e q u i p p e d one At the I. flavor dry b e v e r a g e 105 g o f c u b e d in crystalline pure crystals and about including molecular low-calorie, and e s s e n t i a l l y dry of the weight a dry, The dry mix was p l a c e d a CO2-loaded, sumption, parts 15.9 ounce). Fig. beverage about fluid fluid 6.7 of servings substantially with crystals 10.6 of parts fructose This sample illustrated point-of tap w a t e r con- added. A panel of beverages. The p a n e l i s t a sweetness scale Table mix I under of in II. cool the ice cubed 105 g of from the disc on in beverage B was II Example When s e r v e d , t h e a serving and a CO2-loaded column mix of beverage into two beverage low-calorie dry a day b e f o r e . was poured tasted beverages, shown shown under beverage same dry water tap the test of each sweetness One of 90. The o t h e r solution one-day-old the A, was made by d i s s o l v i n g 200 ml of rated 10 to column Example prepared of in a b l i n d casters expert for cup c o n t a i n i n g a 10.6 fluid ounce serving. The mix the dry tap water The beverage each The b e v e r a g e s , about 6.0 about 4 minutes ef fluid per before in both carbonation volumes of was found bevorage under was about of approaching approaching 90 are unacceptable with It the will be noted sweetness rating scale. of cool stand to 4 minutes, about 1.5 to of for the about level 1.6 liquid. of level the be g r e a t e r to under beverage than that column A of the B. On a s w e e t n e s s ratings content allowed were beverages panelists column serving, 200 ml of and a caloric having from prepared carbonated. rapidly After sweetness by a l l is tasting. volume CO2 per The of ounce ice 105 g of cubed about by adding thereto. column A was f r e s h l y under beverage scale of the least 10 are the most the from Table Beverage level I that A near of the the as used sweet, with sweet, optimum 10-90 both in Table whereas ratings extremes sweetness average I, being panelist optimum m i d - p o i n t being about 50. rated of the . EXAMPLE I I I A 2000 g batch carbonated cola of a dry low-calorie mix was p r e p a r e d beverage dietetic the having following formulation: The dry mix was p r e p a r e d dry with ingredients the cola liquid resulted flavor in a uniform mixed with wet f l a v o r - c o a t e d was passed Standard sweetener and vacuum-dried a U.S. to provide screen coated with said The dry beverage having a CO2-loaded Patent 4,007,134, 105 g of ice with the promote disc the carbonation. Fig. 3, and dry mix, dissolution disc the into shelf The d r i e d product on a U.S. #18 fructose the into serving as d e s c r i b e d a level the fluid ounce cup making C02 d i s c h a r g e d was r a p i d l y cups in U.S. of 17.5 g; about serving. contact to a g i t a t e a n d of the dry mix and provide The beverage tem- and a c i d u l a n t . to make a 1 1 . 3 was i n t r o d u c e d a uniform at a drying mix was packed at admixture This wet mass was a combination of supra, This was t h e n and r e t a i n e d flavorant admixture until and 100°F. #6 screen carbonation was added When the water blender mass r e s u l t e d . room t e m p e r a t u r e through The s l u r r y slurry. the the combining and a c i d u l a n t . in a Hobart fructose to t r a y s between perature and then base liquid fructose the transferred first together and mixing by weighing carbonated. beverage The b e v e r a g e of e x p e r t minutes; a panel dietetic carbonated and w i t h o u t a n y was allowed tasters beverage unpleasant to stand tasted and found aftertaste. it for about the 5 fructose-sweetened acceptably sweet A dry, l o w - c a l o r i e c a r b o n a t e d beverage mix comprising a s w e e t e n e r , a f l a v o r a n t , an a c i d u l a n t and an i n s t a n t c a r b o n a t i o n device e f f e c t i v e to c a r b o n a t e a beverage when said mix is brought into c o n t a c t with a 1. beverage-making l i q u i d , c h a r a c t e r i s e d in t h a t the b e v e r a g e is free of a r t i f i c i a l sweeteners and in t h a t the s w e e t e n e r comprises e s s e n t i a l l y pure f r u c t o s e which p r o v i d e s s u b s t a n t i a l l y all of the c a l o r i e s . 2. A beverage mix according to Claim 1 c h a r a c t e r i s e d in t h a t the i n s t a n t c a r b o n a t i o n device is a C 0 2 - l o a d e d m o l e c u l a r sieve d e v i c e . A beverage mix according to Claim 1 or Claim 2 3. c h a r a c t e r i s e d in t h a t the i n s t a n t c a r b o n a t i o n device i s a s i n g l e molded block having a t h i c k n e s s of from a b o u t 0.001 inch to about 3 i n c h e s ; said block being a f f i x e d in said c o n t a i n e r , whereby when said b e v e r a g e - m a k i n g l i q u i d is i n t r o d u c e d in said c o n t a i n e r making c o n t a c t with said mix and said block, said C02 is d i s c h a r g e d t o a g i t a t e and promote d i s s o l u t i o n of said dry mix and p r o vide beverage c a r b o n a t i o n . 4. A beverage mix according to any one of Claims 1-3 c h a r a c t e r i s e d in t h a t the beverage mix comprises d r y f l a v o r c r y s t a l s comprising the f l a v o r a n t , the a c i d u l a n t , and a c r y s t a l l i n e sugar c a r r i e r . A beverage mix a c c o r d i n g to Claim 4 c h a r a c t e r i s e d the f l a v o r c r y s t a l s c o n s t i t u t e from 4% to 12% by weight of the dry beverage mix, and in t h a t the c r y s t a l l i n e sugar c a r r i e r is sucrose which c o n s t i t u t e s from about 20% to 50%.by weight of the dry f l a v o r c r y s t a l s . 5. in t h a t of making a sweet, f l a v o r e d c a r b o n a t e d beverage comprising adding a beverage-making l i q u i d to a sweetened dry beverage mix at the point of c o n s u m p t i o n , said beverage mix comprising a s w e e t e n e r , a f l a v o r a n t , an a c i d u l a n t and an i n s t a n t c a r b o n a t i o n device e f f e c t i v e to c a r b o n a t e the beverage at the point of c o n s u m p t i o n when said b e v e r a g e - m a k i n g l i q u i d i s . a d d e d to said b e v e r a g e c h a r a c t e r i s e d in t h a t the sweetener comprises n o t mix, 6. A method less 88% by weight of t o t a l sweetener of e s s e n t i a l l y pure c r y s t a l l i n e f r u c t o s e whereby said sweet, f l a v o r e d c a r b o n a t e d beverage has a sweetness l e v e l g r e a t e r t h a n the sweetness l e v e l of a c a r b o n a t e d beverage s w e e t e n e d with p r e d i s s o l v e d f r u c t o s e on a c a l o r i e - f o r - c a l o r i e b a s i s . than 7 . ' A method a c c o r d i n g to Claim 6 c h a r a c t e r i s e d i n t h a t the i n s t a n t c a r b o n a t i o n device comprises a CO2loaded m o l e c u l a r sieve device and in t h a t the c a r b o n a t e d . beverage has a more rapid r a t e of c a r b o n a t i o n at t h e point of consumption than has a c a r b o n a t e d b e v e r a g e sweetened with s u c r o s e and c a r b o n a t e d with the s a i d instant carbonation device. A method a c c o r d i n g to Claim 6 or Claim 7 8. c h a r a c t e r i s e d in t h a t the beverage mix comprises d r y f l a v o r c r y s t a l s c o m p r i s i n g said a c i d u l a n t and said f l a v o r a n t and a c r y s t a l l i n e sugar c a r r i e r . 9 . A method a c c o r d i n g to Claim 8, c h a r a c t e r i s e d i n t h a t the c r y s t a l l i n e sugar c a r r i e r is s u c r o s e , in t h a t the c a r r i e r is from 20% to 50% by weight of the f l a v o r c r y s t a l s , and in t h a t the f l a v o r c r y s t a l s c o n s t i t u t e from 4% to 12% by weight of said dry beverage mix.
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