Abstract: A method was developed for the determination of 30 volatile organic compounds (including acetone, benzene, 1-methoxy-2-propanol and 2-ethoxyethanol, etc.) in leather by static headspace gas chromatography-mass spectrometer(HS-GC-MS). The effects of headspace equilibrium temperature and equilibrium time on abundance of analytes were investigated respectively. The 30 VOCs were scanned in selective ion mode(SIM), conducted by mass spectrometry detector, and the contents were calculated by the matrix correction and external standard method. The results showed that VOCs were well quantitatively analyzed while the headspace equilibrium temperature at 120 ℃ for 40 min with the sample diameter 0.5 cm × 0.5 cm. The calibration curves were linear in the range of 0.5 -50.0 μg with the correlation coefficients of each substance more than 0.999. The limits of detection were 0.05 - 0.50 mg/kg. The average recovery rate ranged from 82.0% to 104.2%, and the relative standard deviations(n=6) were 1.7% - 9.8%. This method could be suitable for the determination of 30 VOCs in leather rapidly and accurately.