Abstract: A method for the determination of 17 organotin compounds in footwear materials by gas chromatography-mass spectrometry (GC-MS) was developed using external standard in this article. The gas chromatography-mass spectrometry for qualitative and quantitative analysis after ultrasound-assisted extraction with methanol/ethanol mixed solution and derivatization with sodium tetraethyl borate have been used. Experiments show that 17 organotin compounds can be accurately detected by changing the extraction conditions of organic phase and the chromatographic conditions of gas chromatography-mass spectrometry (GC-MS) on the basis of canceling the original internal standard substances.