A rapid, sensitive and accurate matrix solid phase dispersion-accelerated solvent extraction (MSPD-ASE) method for selective determination of sixteen organochlorine pesticide (OCP) residues in fish samples has been developed and validated. 2 g fresh fish muscle was dispersed with 10 g anhydrous sodium sulfate and 2 g acid alumina thoroughly, and loaded into the stainless-steel extraction cell containing 6 g of acid alumina and 10 g anhydrous sodium sulfate. The temperature 60°C and two extraction cycles of 5 min gave adequate extraction efficiency using DCM-hexane (3:7, v/v) mixture as solvent. Not only the lipids, but also other co-extracts, which peaks mostly located in the forepart of chromatograms and maybe interfere the identification or quantitation of analytes, were eliminated exhaustively, while analytes were extracted selectively. Sixteen OCPs were identified by retention time of standards and quantified using mirex as internal standards. These detected OCPs were confirmed by GC-MS in real samples. The performance of proposed method was evaluated and validated: the detection limits were 0.008-0.05 ng g -1 , relative standard deviations were 1.9-5.0%, and recoveries were 91.0-104.1% spiked at 10 ng g -1 level. The accuracy and precision of proposed method were equal to or better than that of traditional Soxhlet extraction method.