Analytical method for saccharin in foods was developed using gas chromatography/mass spectrometry(GC/MS). Methylation with diazomethane, acetylation with MBTFA, and silylation with MSTFA and MTBSTFA were compared. Methylation of saccharin produced N- methylated saccharin as the major product and O-methylated saccharin as the minor one. Silylation of saccharin with MSTFA and MTBSTFA resulted in the formation of the corresponding O-silylated products, respectively. The derivatization of saccharin was optimized with MSTFA. The ions at m/z 240, 255, and 166 were monitored to characterize saccharin.

Analytical method for synephrine and octopamine in citrus fruits, drinks containing citrus fruit, and human urine was developed using gas chromatography / mass spectrometry(GC/MS). Silylation with MSTFA, acetylation with MBTFA, and trimethylailylation with MSTFA followed by tritluoroacetylation with MBTFA were compared. The selective derivatization of aynephrine and octopamine was optimized with two derivatizing reagents ; MSTFA and MBTFA. The ion at mlz 267 was monitored to characterize the benzyl group of the both compounds. Synephrine was detected in the concentrations of 0.46-1.88 ug/g for citrus fruits and 1.2-8.1 ug/ml for drinks. The urinary excretion data of aynephrine showed the highest concentration at the period of 8-20 hours after drinking orange juices and total amounts of its urinary excretion calculated as a parent compound was 11-14% of a dose during 48 hours. Octopamine was not detected in citrus fruits, drinks, and human urine.