Abstract: A GC/MS method for determining 1-aminonaphthalene,2-aminonaphthalene,3-amino-biphenyl,and 4-amino-biphenyl in cigarette smoke was developed.The cigarette smoke was collected by Cambridge filter pad,then the pad were extracted with 5% HCl,the extract was washed with methyl dichloride,alkalized by sodium hydroxide solution,re-extracted with n-hexane,derived with pentafluoride propionyl anhydride,purified by a Florisil column,and determined by GC/MS with selection ion monitoring mode using d³-2-aminonaphthalene as an internal standard.The results showed that the recoveries of the 4 aromatic amines were over 90% with RSD of below 10% and the limits of detection of below 0.7 ng/mL.The method is suitable for the quantitative analysis of the 4 aromatic amines in cigarette smoke.