[目的] 建立一种生乳中多种农药残留快速定性定量的高效液相色谱串联质谱分析方法。[方法] 生乳样品经乙腈提取后,用含有150 mg N-丙基乙二胺（PSA）、900 mg硫酸镁、15 mg C18净化,后经液相梯度洗脱。在电喷雾（ESI+/ESI-）下使用质谱进行检测,通过基质匹配外标法定量,建立生乳中83 种农药残留快速定性定量分析方法。[结果] 经验证,83 种农药残留在0.5~100 μg/L范围内线性良好,相关系数R2>0.99。在 3 水平添加（0.010 mg/L、0.020 mg/L、0.100 mg/L）回收率为32%~134%,相对标准偏差为0.3%~8.5%。[结论] 该试验方法操作简单、耗时短,适用于生乳中农药残留快速筛查和定量分析,具有实际应用价值。用该方法检测50 批次生乳中83 种农药残留,均满足《GB 2763—2021 食品安全国家标准 食品中农药最大残留限量》对生乳的要求。
[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.
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