A gas chromatography-mass spectrometric(GC-MS) method was developed for the determination of 16 organotin compounds in textile materials and their products.Samples were ultrasonically extracted with a mixture of methanol and sodium acetate,then the extract was derived with sodium tetraethyl borate,and extracted with n-hexane.The target ingredients were separated on a DB-5MS(30 m×0.25 mm×0.25 μm) column.The 16 organotin compounds were analyzed in selective ion mode(SIM).Under the optimal conditions,the calibration curves for 16 organotin compounds were linear in the range of 50-500 μg/L,with limit of quantitation of 0.05 mg/L(0.15 mg/kg).The recoveries ranged from 77.6%to 106.0%,with relative standard deviations(RSDs,n=6) not more than 8.3%.This method was rapid,reliable,accurate and convenient to operate,and it was appropriate for the determination of organotin compounds in textile materials and their products in routine tests.