Abstract: A microwave assisted extraction-solid phase extraction-gas chromatography-tandem mass spectrometry (MAE-SPE-GC-MS/MS ) method for the determination of 17 kinds of PCBs in fishery product was developed. The fishery product samples were extracted with the solution （V（n-hexane）∶V（acetone）=1∶1） by microwave assisted extraction technique. Clean-up was carried out with florisil solid phase extraction. After HP5-MS chromatographic column separation using helium as a carrier gas, the eluents were determined under multi-reaction monitoring (MRM) scan type with tandem mass analyzer. The correlation coefficients are larger than 0.999， and the limit of quantification (LOD) is 0.5—1.0 μg/kg. At the spiked levels of 5.0, 10.0, 20.0 μg/kg, the average recoveries range from 83.1% to 100.8%, and the relative standard deviations(RSDs) range from 4.36% to 9.38%. The proposed method had been used for the determination of 17 kinds of PCBs in complex sample.