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A method for rapid determination of 95 kinds of pesticide residues in agricultural products by solvent extraction, GPC clean-up and GC/MS-SIM was developed. 1) A mixed solvent of acetone-ethyl acetate-n-hexane (2:9:9) was selected for extraction, with anhydrous sodium sulfate as a drying agent. 2) GPC elution profiles of pesticides and major components in agricultural products were studied with various organic solvents, i. e., toluene, dichloromethane, ethyl acetate, tetrahydrofuran and cyclohexane. Toluene was selected as the most suitable mobile phase for GPC with well-swollen Bio Beads S-X3. 3) Detection limits of 95 pesticides by GC/MS-SIM were sufficient for practical use. Eighty-six pesticides spiked into 5 kinds of agricultural products gave good recoveries by the proposed method, which is considered to be satisfactory for the rapid determination of multiple pesticide residues in agricultural products.