Abstract: The sample (0.500 0 g) was added in to 10 mL of deionized water, and the mixture was shaken for 15 min to make the water fully infiltrate the sample. Then 10 mL of ethanol, 500 μL of mixed internal standard solution containing 100 mg·L^-1 D4-dibutyl phthalate and 28 mg·L^-1 2,4,6-tribromobiphenyl were added, and the mixtrue was ultrasonically extracted for 30 min. After adding 4 g of MgSO₄, 1 g of NaCl, the mixture was vortexed. Then 2 mL of supernatant was taken, and 5 mL of a mixture of n-hexane-ethyl acetate (3+2) was added for liquid-liquid extraction. 18 kinds of phthalate esters, tributyl phosphate, and 7 kinds of polychlorinated biphenyls in the extract were separated on a DB-5MS UI capillary column (30 m×0.25 mm, 0.25 μm). Electron bombardment ion source and selective ion monitoring mode were selected in MS analysis. The ratios of the peak areas of the 26 compounds to the peak areas of the internal standards were linear with the corresponding rations of mass concentrations within definite ranges, and the detection limits (3S/N) were in the range of 0.010-2.558 mg·kg^-1. Values of recovery obtained by standard addition method ranged from 85.1% to 102%, and RSDs (n=6) were less than 9.0%.