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Open AccessArticle10.2478/cttr-2013-0930

Trace Analysis of Mutagenic Heterocyclic Aromatic Amines in Cigarette Smoke Condensate and its Base Fractions via Silylation-GC-MS

S Liu,L. T. Taylor,MF Borgerding,W. Emile Coleman,BR Bombick-2013-03-01-Beiträge zur Tabakforschung international
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Abstract Among the more than 5000 chemicals reported in cigarette smoke condensate (CSC), heterocyclic aromatic amines (HAAs) are considered to be a contributor to observed biological activity. HAAs are non-volatile and are reported at ppb levels in CSC. A new method for HAA analysis at the trace level is reported here. N, O-Bis(trimethylsilyl) trifluoroacetamide (BSTFA) containing 1% trimethylchlorosilane was employed to derivatize amino groups by heating the reagent containing a sample of CSC at 80 °C for 30 min followed by analysis employing gas chromatography-mass spectroscopy (GC-MS) in the selected-ion-monitoring (SIM) mode. This derivatization method afforded symmetrical peak shapes on a ZB-50 stationary phase and achieved instrumental limits of quantification (LOQ) at 10:1 S/N from -1 ng/mL for AαC to120 ng/mL for Glu-P-1. The chemical identity of each derivative was confirmed by comparison of retention time and mass spectra of standards. The latter were characterized by the fo

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Abstract Among the more than 5000 chemicals reported in cigarette smoke condensate (CSC), heterocyclic aromatic amines (HAAs) are considered to be a contributor to observed biological activity. HAAs are non-volatile and are reported at ppb levels in CSC. A new method for HAA analysis at the trace level is reported here. N, O-Bis(trimethylsilyl) trifluoroacetamide (BSTFA) containing 1% trimethylchlorosilane was employed to derivatize amino groups by heating the reagent containing a sample of CSC at 80 °C for 30 min followed by analysis employing gas chromatography-mass spectroscopy (GC-MS) in the selected-ion-monitoring (SIM) mode. This derivatization method afforded symmetrical peak shapes on a ZB-50 stationary phase and achieved instrumental limits of quantification (LOQ) at 10:1 S/N from -1 ng/mL for AαC to120 ng/mL for Glu-P-1. The chemical identity of each derivative was confirmed by comparison of retention time and mass spectra of standards. The latter were characterized by the fo

Keywords

ChemistryBSTFADerivatizationSilylationTrimethylsilylChromatographyReagentMass spectrum

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