| A method was developed for the simultaneous determination of 15 phthalic acid esters at trace level in aquatic products by solid phase extraction（SPE） purification coupled with gas chromatography-mass spectrometry（GC-MS）.The PAEs were extracted with dichloromethane-hexane（1∶1） by ultrasonic-assisted technique,then purified with SPE glass column packed with 3.0 g neutral alumina caped with approximately 2 cm anhydrous sodium sulfate on the top. The target analytes were eluted with hexane,dichloromethane-hexane（1∶9） mixture,ethyl acetate-hexane（1∶4）mixture,and ethyl acetate,sequentially.The eluent was evaporated to near dryness,and redissolved in 1 mL hexane,and analyzed by GC-MS under the selected ion monitoring mode.Under optimized conditions,the linear ranges of 15 phthalic acid esters were in the range of 0.05-1.0 mg/L with correlation coefficients（r） not less than 0.999 1.The average recoveries of 15 phthalic acid esters in different kinds of fishery products samples at spiked levels of 2,50,200 μg/kg were in the range of 81%-123%,with relative standard deviations（RSDs,n=3） less than 15%.The limits of detection（LOD,S/N=3） ranged from 0.04 μg/kg to 1.18 μg/kg,and the limits of quantitation（LOQ,S/N=10） ranged from 0.20 μg/kg to 4.00 μg/kg.The proposed method is suitable for the simultaneous determination of 15 phthalic acid esters in fishery products with easy operation,high accuracy and precision. |