Abstract: A sensitive and precise method for determination the content of free nicotine in total particulate matter of cigarette-smoke by gas chromatographic means was established. The anethole is used as internal standard, the capillary column is a HP-INNOWAX(30 m×0.25 mm I.d×0.25 μm) and the detector is FID. A good linearity was obtained from 6.56 μg/mL to 22.96 μg/mL(r=0.999 45). The average recovery was 95.42%.