GLC-mass fragmentographic determination of saccharin in biological fluids.

A specific and sensitive method is described for the determination of saccharin in biological fluids. The compound is extracted as its methyl derivative following a salt-solvent pair procedure and assayed by GLC with either flame-ionization or mass fragmentographic detection using ethylated or trideuteromethylated saccharin, respectively, as the internal standard for quantitation. Detector response was linear over concentrations of 50 mg/ml--10 micrograms/ml with multiple-ion detection mass fragmentography and from 2 micrograms/ml up to milligram levels with flame-ionization detection. Interference from endogenous substrates was never observed. Plasma kinetics and urinary elimination of saccharin in healthy human volunteers given the sweetener orally, acutely (50 mg/60 kg of body weight) or for 5 days (130 mg/60 kg of body weight/day divided over the three main meals), also are reported.