Acesulfame sample preparation

Two main standards were developed, one for the sweeteners showing UV absorption, i.e. acesulfame, aspartame and saccharin,36 and a separate standard for cyclamate37 which does not show a substantial UV absorption. Both standards use HPLC and propose specific sample preparation procedures. HPLC is also the suitable technique for the quantitative determination of sucralose.38... 

Sample preparation for HPLC analysis of acesulfame-K can be accomplished as described in Sec. I.C. A number of extraction procedures for acesulfame-K have been reported (16,17,33,34,40,44,49). Sodium fumarate and theophyllin can be used as internal standard (17,44). 

Procedure Separately inject equal 20-p.L portions of the Standard Preparation and the Sample Preparation into the chromatograph, and record the chromatograms for a time equal to twice the retention time of Aspartame. In the chromatogram obtained from the Sample Preparation, the sum of the responses of all secondary peaks, other than those for 5-benzyl-3,6-dioxo-2-piperazineacetic acid and Acesulfame, is not more than the response of the Aspartame peak obtained in the chromatogram from the Standard Preparation. Potassium... 

The test identifies the substance to be examined as a salt of potassium, K+. As with other alkali metals, potassium is exclusively found as the monovalent cation. Since almost all salts of potassium are water soluble and it is a very inert ion, as a rule these do not contribute to the characteristics of its salt. For this reason its function in the compounds enrolled in the pharmacopoeia is to be an indifferent counter-ion, both for simple inorganic anions but also for anionic active pharmaceutical ingredients. Reference to potassium is made in about twenty-five monographs. In about half of them test (b) is dictated in about one-quarter and in the last quarter both tests have to be performed. The anions in the organic salts are, with the exception of Acesulfame, carboxylic acids. Due to the high water solubility of potassium, sample preparation is in most cases just a simple dilution in water. 

Optical (Specific) Rotation Determine as directed under Optical (Specific) Rotation, Appendix HB, using a solution containing 6.2 g of sample in sufficient 15 N formic acid to make 100 mL. Make the determination within 30 min of preparation of the Sample Solution. Divide the calculated specific rotation by 0.646 to correct for the Aspartame content in Aspartame-Acesulfame Salt. 

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