A method based on high performance liquid chromatography-hydride generation-atomic fluorescence spectrometry（HPLC-HG-AFS） for simultaneous determination of organotin compounds,e.g.dimethyltin（DMT）,trimethyltin（TMT） and diphenyltin（DPhT） in plastic samples was established.Various experimental parameters were optimized.DMT,TMT and DPhT were chromatographically separated on an Agela-C18 column by using mobile phase of methanol-water-acetic acid-triethylamine（60∶40∶1∶0.03） at a flow rate of 0.7 mL?min-1.The hydrogenation of organotin compounds reacted in the environment of 5% HCl and 2% KBH4.The different concentration mixed organotin compounds（DMT,TMT and DPhT） standard were tested.The experimental results indicated that the calibration curves were linear in the range of 10-200 μg/L with correlation coefficients（r） more than 0.992.Different plastic samples were dissolved completely in tetrahydrofuran（THF）,the impurities of high molecular weight were deposited by mixing methanol in THF solutions.The solutions were tested by HPLC-HG-AFS after high speed centrifugation and filtration.The average recoveries of DMT,TMT and DPhT in PVC,PC,PS,AS and ABS samples ranged from 75.1% to 109.1%,with relative standard deviations of 3.7%-10.7%.The detection limits of DMT,TMT and DPhT were 0.009 ,0.012 mg/kg and 0.025 mg/kg,respectively.