关键词: 高效液相色谱串联质谱, 农药残留, 生乳

Abstract: [Objective] To establish a high-performance liquid chromatography tandem mass spectrometry analysis method for multiple pesticide residues in raw milk.[Method] Raw milk samples were extracted with acetonitrile,purified with 150 mg of N-propylethylenediamine（PSA）,900 mg of magnesium sulfate and 15 mg of C18,and then eluted with liquid phase gradient.The samples were detected by electric spray（ESI+/ESI-）,and quantified by matrix matching external standard method.A rapid qualitative and quantitative analysis method for 83 pesticide residues in raw milk was established.[Result] The results of method validation showed that 83 pesticide residues exhibited good linearity within the range of 0.5 μg/L to 100 μg/L,with a correlation coefficient R²>0.99.The recovery rate of adding at three levels（0.010 mg/L,0.020 mg/L,0.100 mg/L） is 32%~134%,with a relative standard deviation of 0.3%~8.5%.[Conclusion] This experimental method is simple to operate,time-consuming,and suitable for rapid screening and quantitative analysis of pesticide residues in raw milk.It has practical application value. Using this method,83 pesticide residues were detected in 50 batches of raw milk,all of which meet the requirements of the GB 2763—2021 National Food Safety Standard Maximum Residue Limits for Pesticides in Food for raw milk.

Key words: HPLC-MS/MS, pesticide residue, raw milk