Abstract: A method for determination of 9 triazine herbicides residues in aquatic products by gel permeation chromatography-solid phase extraction-gas chromatography tandem mass spectrometry(GPC-SPE-GC-MS/MS) was established. The sample was extracted with ethyl acetate, then cleaned up by gel permeation chromatography and purified by carbon and NH₂ solid phase extraction column. The analytes were determined in selected ion monitoring and quantified by external method. Propazine, atrazine, terbuthylazine, simazine and cyprazine show good linearity in the range of 1.0-50.0 μg/L, and the detection limits of the five analytes are 1.0 μg/kg. The average recoveries range from 86.3% to 119% when spiked at 1.0-10.0 μg/kg with relative standard deviations from 5.11% to 10.1%. Simetryn, prometryn, ametryn and terbutryn show good linearity in the range of 2.0-100.0 μg/L, and the detection limits are 2.0 μg/kg. The average recoveries range from 87.6% to 112% when spiked at 2.0-20.0 μg/kg with relative standard deviations from 5.27% to 9.56%. The method is stable and reasonable, and which can be used for the determination of 9 triazine herbicides residues in aquatic products.