Abstract: A procedure has been developed to determine the migration of organotin compounds in plastic toys by GC-MS method. The organotin compounds were extracted by an 0.07 mol/L hydrochloric acid solution, derivatied with NaBEt4, extracted by hexane, and the quantitative analysis of ethyl organotins was carried out by GC-MS, using an external standard method. The linear calibration curve was obtained in the range of 0.1~7.5 mg/L with a correlation coefficient of >0.9983. The limits of quantification were 0.04~0.16 mg/kg and the average recoveries were in the range of 89.3%~105.4% for 10 organontins with the relative standard deviations <9.7%. The method is simple, rapid, accurate and can be applied to the determination of the migration of orgaontins in plastic toys.