A method was developed for the analysis of 1-nitro-naphthalene, 1-nitropyrene, and 6-nitrochrysene in main stream cigarette smoke, using [14C]1-nitronaphthalene, [14C]1-nitropyrene, and [14C]6-nitrochrysene as tracers and internal standards. Cigarette smoke condensate was collected and the appropriate fractions containing the labelled standards were obtained by a series of solvent partitions and column chromatography. Recovery of internal standards ranged from 60 to 70%. The fractions were analyzed by capillary gas chromatography with electron capture detection and by combined capillary gas chromatography - mass spectrometry. 1-Nitronaphthalene (<10ng/cigarette), 1-ni-tropyrene (<10ng/cigarette), and 6-nitrochrysene (<1ng/cigarette) were not detected in the mainstream smoke of the University of Kentucky 1R1 cigarette, a US commercial 85 mm non-filter cigarette, or a French commercial 70 mm non-filter cigarette.