A dispersive solid phase extraction coupled with gas chromatography-mass spectrometric method was established for the simultaneous determination of sixteen polycyclic aromatic hydrocarbons （PAHs） in fish and shrimp samples.The target analytes in samples were extracted twice with n-hexane-dichloromethane（1∶1,by volume）,followed by Florisil clean-up and sulfuric acid purification.The PAHs were analyzed by GC-MS under selected ion monitor（SIM） mode and quantified by the internal standard method.The procedure of sample pretreatment,the amount of dispersant and the instrument conditions were also optimized in the present study.Under the optimal conditions,good linearities were obtained in the range of 1-200 μg/L for sixteen analyzed compounds with correlation coefficients not less than 0.998 6.The limits of detection（S/N=3） ranged from 0.38 μg/kg to 1.5 μg/kg.The average recoveries of 16 PAHs from the carp and tilapia muscle samples at two spiked levels of 5 μg/kg and 15 μg/kg ranged from 90% to 102% with RSDs of 1.9%-8.5%.The method was simple,rapid and accurate,and could be used for the routine analysis of PAHs in fish and shrimp as well as other aquatic products.