Abstract: To analyze the volatile and semi-volatile components in vapor and particulate phases of mainstream cigarette smoke (MS), the efficiencies of trapping vapor phase components by tandem XAD-2 adsorption tube and 0.01% triethylamine/methanol cool solution and the extraction efficiencies of methanol, dichloromethane, cyclohexane, hexane and ethyl acetate for components trapped by the tandem XAD-2 adsorption tube and Cambridge filter were investigated. The volatile and semi-volatile components in vapor and particulate phases of MS produced by reference cigarettes 3R4F, lR5F and a domestic reference Virginia type cigarette were determined by gas chromatography/mass spectrometry. The results indicated that: 1) the volatile and semi-volatile components in vapor and particulate phases of MS were basically completely trapped by combination of XAD-2 tube and 10 mL 0.01% triethylamine/methanol cool solution (temperature ≤-80℃);2) 0.01% triethylamine/methanol solution was suitable for the extraction of these components;3) 50 components were identified, including 19 aromatic compounds, 14 ketones, 4 pyridines, 6 furans and 7 other compounds;4) the components whose boiling points were over 250℃ or below 80℃ were not detec-table in vapor and particulate phases;5) there were a similar tendency in distribution ratios of volatile and semi-volatile components in vapor phase to particulate phase of MS of 3 reference cigarettes, and the distribution ratios of the same kind of volatile and semi-volatile components and of the different kind of components with similar boiling points in MS decreased with the increase of their boiling points and their polarities, respectively.