Reference

Quantitation of o- and p-sulfamoylbenzoic acids in commercial saccharin by high speed liquid chromatography

Quantitation of o- and p-sulfamoylbenzoic acids in commercial saccharin by high speed liquid chromatography. Nelson, James J. (Food Drug Adm., Publ. Health Serv., New York, N. Y., USA). EDRO SARAP Res. Tech. Rep., 1, Paper 45-74, 25 pp. (English) 1976. CODEN: ESRRD5. DOCUMENT TYPE: Journal CA Section: 17 (Foods) A 6 g saccharin [81-07-2] sample was dissolved in 30 mL MeOH, 1.6 mL HNO3 was added, and the mixt. was chilled and centrifuged. The ppt. was shaken with 10 mL MeOH and centrifuged. The supernatant was dried under N, mixed with 0.2 mL MeOH, and again dried. An internal std. (p-hydroxybenzoate) was added and the material was subjected to high speed liq. chromatog. on a Dupont SAX column with 0.008M NaNO3 in 0.01M Na tetraborate buffer as the mobile phase. O-sulfamoylbenzoic acid [632-24-6] and p-sulfamoylbenzoic acid [138-41-0] were quantitated with a UV detector and were detd. accurately at the 80 and 25 ppm levels, resp. O-toluenesulfonamide [88-19-7], p-toluenesulfonamide [70-55-3], 1,2-benzisothiazoline-1,1-dioxide [936-16-3], and 3-amino-1,2-benzisothiazole S-dioxide [7668-28-2] were extd. from saccharin with Me2CO and detd. with an ODS column with isooctane as the mobile phase.

The fate of saccharin impurities

The fate of saccharin impurities. The excretion and metabolism of [14C]toluene-4-sulfonamide and 4-sulfamoyl[14C]benzoic acid in the rat. Ball, L. M.; Williams, R. T.; Renwick, A. G. (Dep. Biochem., St. Mary's Hosp. Med. Sch., London, Engl.). Xenobiotica, 8(3), 183-90 (English) 1978. CODEN: XENOBH. ISSN: 0049-8254. DOCUMENT TYPE: Journal CA Section: 17 (Foods) Section cross-reference(s): 4 14C-labeled 4-sulfamoylbenzoic acid (I) [138-41-0] (22 mg/kg), an impurity of com. saccharin [81-07-2], was rapidly eliminated after oral administration to rats (94% of dose in 24 h). After 6 days, 73-83% of the dose 14C was recovered in the urine as unchanged I, with 18-32% in the feces due to incomplete absorption. After oral administration of 14C-labeled toluene-4-sulfonamide (II) [70-55-3] (29 mg/kg), another impurity of com. saccharin, to rats, 66-89% of dose was rapidly eliminated in the urine with 2-8% in the feces. The urine of rats given II contained I as the major metabolite (93%) with small amts. of unchanged II (1.5-2.3%), 4-sulfamoylbenzyl alc. [67472-44-0] (2.0-3.9%), 4-sulfamoylbenzaldehyde [3240-35-5] (0-1.5%), and, at a higher dose (200 mg/kg), N-acetyltoluene-4-sulfonamide [1888-33-1] (2.1-2.3%). The label in the feces following II administration was unchanged II.