Analytical method for preservatives in food was developed using gas chromatography/mass spectrometry (GC/MS). Propionic acid, sorbic acid, benzoic acid, ethyl salicylate, ethyl p-hydroxy benzoate, iso-propyl p-hydro benzoate, n-propyl p-hydroxy benzoate, iso-butyl phydroxy benzoate, n-butyl p-hydroxy benzoate, p-hydroxy benzoic acid and dehydro acetic acid were extracted from cooling beverage with diethyl ether. The polar hydroxyl and carboryl groups of food preservatives were derivatized with N-methyl-N-tent-butyldimethylsilyl-trifluoroacetamide (MTBSTFA) to form the corresponding tert-butyldimethyl-silylated derivatives, and submitted to GC/MS analysis. The mass spectra of the derivatives were investigated for the selection of monitoring ions for multi-residue analysis of 11 preservatives by GC/MS. The macro program was also developed for the qualitative analysis of these preservatives in food.

The prevention of oxidative degradation in fats and oils is largely controlled by the use of synthetic phenolic antioxidants. Antioxidants, BHA: 2-&3-tert-butyl-4-hydroxyanisol, BHT: 3,5-di-tert-butyl-4-hydroxytoluene, TBHQ: tert-butylhydroquinone, PG: propyl gallate, PTG: pentyl gallate, OG: octyl gallate, were extracted from fatty foods with hexane and from hexane layer to presaturated acetonitrile with hexane. The polar phenolic hydroxyl groups of antioxidants were silylated with MSTFA and injected to Gas Chromatography/Mass Spectrometry. The calibration plots were linear in the investigated range, 0.1-10.0 ug/g. The limit of detection for 6 phenolic antioxidants was 0.1 ug/g. Recoveries and reproducibilities from samples fortified at 1.0 ug/g were in the range of 70-90% and 0.5-13%, respectively. The simultaneous determination of phenolic antioxidants in fatty foods using GC/MS-SIM mode and macro program was described.

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.