Abstract: An HS-SPME-GC/MS (Headspace solid-phase microextraction-gas chromatography-mass spectrometry) method was developed to analyze selected aroma compounds in the particulate matters of mainstream cigarette smoke. The puff-by-puff release of 8 aroma compounds, including pyridine, pyrrole, furfural, 5-methyl furfural, 3-methylpyridine, D-limonene, 2, 3, 5, 6-tetramethyl pyrazine and β-damascenone were quantitatively determined with this method. The results showed that: 1) The optimal experimental conditions are: extracting with 85 μ m CAR/PDMS SPME column at 60 ℃ for 60 min and desorbing at 250 ℃ for 8 min. These parameters gave the highest SPME efficiency. 2) Under the optimized conditions, the linear correlation coefficients of the calibration curve, relative standard deviations (RSDs) and recoveries of the 8 standard compounds were 0.969 8-0.999 5, 3.8%-9.0% and 78%-105%, respectively. 3) The release of aroma compounds in mainstream smoke during ISO smoking differed from that of nicotine. With each puff, the release of total particulate matter and nicotine in mainstream smoke was increased, while the puff-by-puff yields of the 8 compounds in mainstream smoke were relatively stable.