Patent EA-000281-B1 (EA)
Title: Sweetener salts
Inventor: FRAY JOHN CHARLES
IPC: A23L27/30
Filed: 1996-10-10
Abstract: 1. Process for the preparation in a liquid medium of sweetening salts consisting of two sweetener components, starting from a sweetener derived from aspartic acid and a derivative of an organic sweetening acid which corresponds to an intense sweetener not derived from aspartic acid, characterized in that the following are added to the liguid medium, in any order of the steps (a), (b) and (c): a) as component (i) the sweetener derived from aspartic acid; b) as component (ii) a salt of an organic sweetening acid which corresponds to an intense sweetener not derived from aspartic acid; c) as component (III) a strong acid; d) the components then present in the system are allowed, optionally with agitation, to react for at least one minute, upon which the sweetening salt is formed; and e) the sweetening salt is isolated from the resulting reaction mixture. 2. Process according to Claim 1, characterized in that, at least at the end of step (d); at least 1.0 wt.% of solid material is present in the reaction mixture. 3. Process according to Claim 1, characterized in that the sweetener derived from aspartic acid and the salt of the organic acid which corresponds to an intense sweetener not derived from aspartic acid are applied in a molar ratio in the range from 0.2:1 to 5:1, in particular in the range from 0.5:1 to 2:1. 4. Process according to any one of Claims 1-3, characterized in that the sweetener derived from aspartic acid and the salt of the organic acid which corresponds to an intense sweetener not derived from aspartic acid are applied in a molar ratio of about 1:1. 5. Process according to any one of Claims 1-4, characterized in that the liquid medium is chosen from the group formed by water, polar organic solvents, apolar organic solventsand mixtures thereof as well as water-miscible or water-immiscible solvent blends, and mixtures with components of the above-mentioned liquids, including aqueous media. 6. Process according to Claim 5, characterized in the liquid medium is an aqueous medium, in particular water. 7. Process according to any one of Claims 1-6, characterized in that the strong acid has been chosen from the group formed by hydrochloric acid, sulphuric acid or phosphoric acid, and that the acid used in (c) is applied in the form of a solution, concentrated or not, if the acid is hydrochloric acid, as gaseous HC1. 8. Process according to any one of Claims 1-7, characterized in that the total molar quantity of ion H* of the strong acid is at least equal to 25% of the molar quantity of, and in particular is equimolar to, the sweetener derived from aspartic acid. 9. Process according to any one of Claims 1-8, characterized in that the reaction of the components in step (d) takes place while agitation is being applied. 10. Process according to any one of Claims 1-9, characterized in that one or two of the three components (i), (ii) and (iii) are added to the liquid medium and subsequently the component(s) not yet present is (are) added. 11. Process according to Claim 10, characterized in that the addition of the component(s) not yet present is carried out gradually. 12. Process according to either of Claim 10 or 11, characterized in that use is made of a salt of component (i) with a strong acid when adding the components (i) and (iii) to an aqueous medium. 13. Process according to either of Claim 10 or 11, characterized in that the salt of the organic sweetening acid that is used in step (b) is prepared in situ by allowing the organic sweetening acid to react with a base. 14. Process according to any one of Claims 1-11, characterized in that at least a part of the strong acid is added in step (c), and during step (d) gradual addition of strong acid is continued. 15. Process according to any one of Claims 1-14, characterized in that the reaction of the components in step (d) is carried out at elevated temperature, in particular in the 40-70 degree C range, and the system obtained is subsequently gradually cooled down to a temperature in the 0-20 degree C range. 16. Process according to any one of Claims 1-15, characterized in that the sweetening salt is isolated in step (e) by separating or by crystallizing out and separating the sweetening salt in a known manner from the liquid medium after separation of any inorganic salt. 17. Process according to any one of Claims 1-16, characterized in that the sweetening salt isolated in step (e) is subsequently washed and dried and is optionally recrystallized and/or purified. 18. Process according to any one of Claims 1-17, characterized in that the salt of the organic acid which corresponds to an intense sweetener not derived from aspartic acid has been chosen from the group formed by potassium, sodium, calcium, ammonium and secondary or tertiary amine salts. 19. Process according to any one of Claims 1-18, characterized in that the sweetener derived from aspartic acid is aspartame or alitame. 20. Process according to any one of Claims 1-19, characterized in that the organic acid which corresponds to an intense sweetener not derived from aspartic acid has been chosen from the group formed by acesulfamic acid, saccharinic acid or cyclamic acid. 21. Sweetening salt, consisting of aspartame and acesulfamic acid, with less than 0.5% degradation when heated for 60 minutes at 120 degree C, or less than 0.5% degradation when heated for 70 hours at 70 degree C, and with a moisture content < 0.5 wt.%, in particular < 0.2 wt.%. 22. Crystal modification of a sweetening salt according to Claim 21 of aspartame and acesulfamic acid, characterized by the presence of characteristic X-ray diffraction lines at D-values of about 11.8, 6.04 and 5.02, and by the absence of intense lines at D-values of 13.5 and 6.76 (measured by X-ray diffractometry using Cu-Kα radiation 23. Use of a sweetening salt prepared according to the process of any one of Claims 1-20 or of a sweetening salt according to either of Claims 21 or 22 in foodstuff compositions, confectionery, sweets or chewing gums. 24. Use of a crystal modification of a sweetening salt of aspartame and acesulfamic acid according to Claim 22 in foodstuff compositions, confectionery, sweets or chewing gums, in particular in confectionery. 25. Preparations of sweetening salts according to either of Claims 21 or 22