Abstract: A method of gas chromatography-mass spectrometry (GC/MS) was developed for the simultaneous determination of 9 organic solvent residues in textile and leather, induding ethylene glycol diethyl ether(CET), 2-methoxyethanol (2-ME), 2-ethoxyethanol (2-EE), ethylene glycol monoethyl ether acetate (CAC), N,N-dimethylformamide (DMF), N,N-dimethylacetamide (DMAc), 1,2,3-trichloropropane (TCP), N-methylpyrrolidone (NMP) and triethylene glycol dimethyl ether (TCE). Samples were extracted by methanol, and directly qualitative and quantitative analysis by optimized GC/MS. The results show that calibration curves of 9 organic residues have good linearity with the correlation coefficients not less than 0.9995, and the method detection limits range from 0.12 to 0.23 mg/kg. Using negative cotton, linen, silk and leather as the sample matrix, the recoveries of 9 organic solvents spiked at three levels range from 81.5% to 97.1%, and the relative standard deviations are less than 5.1%. This method is simple and time-saving with high sensitivity and reproducibility, as well as having practical application value.