Supercritical fluid extraction and gas chromatography mass spectrometry for the analysis of tobacco-specific nitrosamines in cigarettes

A method for measuring four tobacco-specific nitrosamines (TSNAs), an impor tant group of compounds in tobacco products, was developed: These compounds were extracted using supercritical fluid extraction (SFE) and purified by a sodium hydroxide wash of the ethyl acetate eluting solvent and solid-phas e extraction. Quantitation was performed using gas chromatography/mass spec trometry (GC/MS). Spiking experiments were carried out to determine the rec overy, precision, and limits of detection of this method. The detection lim its were 0.04 mu g per sample for N '-nitrosonornicotine and N '-nitrosoana tabine and 0.02 mu g for 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone and N'-nitrosoanabine. This method was used to measure TSNAs in various brands of cigarette tobacco with excellent reproducibility. The variation of TSNA levels among the cigarettes of different packs and types was significantly smaller than that among different brands, Comparable TSNA levels were obta ined with SFE and liquid extraction methods. Signal to-noise levels were si milar for GC/MS and GC/thermal energy analysis when low-level tobacco sampl es were analyzed.