Abstract: The content of diisohexyl phthalate in leather products was determined by ultrasonic extraction-assisted gas chromatography-mass spectrometry (GC-MS). Using n-hexane as the solvent, the ultrasonic treatment was conducted at 50 ℃ to extract diisohexyl phthalate from leather products. The GC-MS analysis was then carried out, and the quantitative tests were conducted by external standard method. Results show that, when the range of determination was 1~50 mg/L, the quantitation limit of diisohexyl phthalate was 25 mg/kg, and the spiked average recoveries ranged from 96% to 102%, while the relative standard deviation (RSD) is less than 2% (n = 8). The present method is suitable for the determination of diisohexyl phthalate in leather products.