Abstract:A rapid method for the batch analysis of organochlorine and chrysanthemum ester pesticides in aquatic productions was established by gel permeation chromatography and gas chromatography -triple quadrupole-tandem mass spectrometry （GC-MS/MS），the extraction solvent of sample is optimized，GPC was employed to purify sample combined with dispersive solid-phase extraction （d-SPE），The optimal time for gathering samples were obtained as well as amount of PSA solid-phase extraction adsorbent for sample purification，detected by multiple reaction monitoring mode via electron impact ion source，the limits of detection of the pesticides in aquatic product was between 0.03 μg/kg-2.87 μg/kg，The experimental results showed that The average recoveries of pesticides varied from 60.5 % to 118 %，and the relative standard deviations were between 0.75%and 15%.The method had good reproducibility，high precision，therefore，it was suitable for the detection of a Multi-pesticide residues in loach and other aquatic products.