Abstract: The gas chromatography-mass spectrometry (GC-MS) was used for simultaneous determination of 9 organotin compounds in textiles, which involved liquid-liquid extraction of organotin compounds from textiles, derivatization with NaBEt_4 and analysis of the ethyl organotin by GC-MS in scan mode and selective ion mode. The linearity response of all organotin compounds were well and R2≥ 0.999 0. The average recovery was in the range from 80% to 120% and the RSD was below 7.5%. The detection limit ranged from 0.003 9 mg/kg to 0.075 3 mg/kg. The proposed method has been successfully applied to the determination of organotin compounds in textiles with satisfactory results.