Abstract:To establish an on-line GPC-GC-MS analytic method to determine 17 pesticide residues simultaneously and rapidly in animal derived foods including pork, egg, milk and fat.Methods The pesticide residues were extracted from samples with acetonitrile assisted by n-hexane, salting-out with NaCl and separated through acentric. The supernatant liquid was cleaned up by SPE (NH2), and detected with on-line GPC-GC-MS system. Results The calibration curves of 17 pesticide residues were linear in the range of 0.85-30 μg/L with correlation coefficients above 0.95. The recoveries of the method ranged from 61.2% to 126%. The limits of detection and the limits of quantification were 0.25-3.00 μg/L (S/N≥3) and 0.85-10.0 μg/L (S/N≥10). Conclusion The method was effective, rapid, sensitive, and suitable for the monitoring of the maximum residue limits (MRLs) of 17 pesticide residues in animal derived foods.