The work aims to establish a GAS Chromatogram-Mass-Mass Spectrometer, GC/MS) analysis method to determine the concentration of 10 phthalate esters (PAEs) in printing raw and auxiliary materials. After ultrasonic extraction of tetrahydrofuran and precipitation of acetonitrile, the samples were qualitatively determined by retention time and ions selected. The data were analyzed by the external standard method and GC/MS was used for data analysis. The results showed that the linear range of the 10 PAEs was around 0.05-20 mg/L, and the correlation coefficients were more than 0.999, the quantitation limit of PAEs was 0.003-0.025 mg/kg, and the spiked average recoveries which were obtained from the measures was ranged from 87.12%-123.50%, while the relative standard deviation (RSD) was less than 5%. Such method is obviously easy and flexible, and at the same time the recovery rate is slightly improved than conventional methods, it's particularly suitable for the determination of PAEs in printed raw and auxiliary materials.