固相萃取-气相色谱串联质谱法检测牛奶中41种农药残留

Simultaneous Determination of 41 Pesticide Residues in Milk by Solid-phase Extraction and Gas Chromatography-tandem Mass Spectrometry

目的建立固相萃取-气相色谱串联质谱法(SPE-GC-MS/MS)同时测定牛奶中41种农药残留分析方法。方法采用固相萃取方法对样品进行前处理。样品经乙腈提取、盐析后,提取液经Captiva EMR-Lipid固相萃取柱净化后上机测定。用气相色谱-三重四极杆串联质谱仪进行多农残检测。结果41种农药在50~1000 ng/ml之间呈良好的线性关系,相关系数r均大于0.99。在0.02,0.1,0.2 mg/kg加标水平下,41种农药的平均回收率为60.6%~110.6%,相对标准偏差(RSD)为1.3%~16.6%(n=6)。结论该方法选择性好,操作简单安全,快速准确,适用于牛奶中多种农药残留的测定。

Objective To establish a method for the simultaneous determination of 41 pesticide residues in milk by solidphase extraction and gas chromatography-tandem mass spectrometry.Methods The sample was pretreated by solidphase extraction.The sample was extracted with acetonitrile,and after salt extraction,the extracting solution was purified by Captiva EMR-Lipid solid-phase extraction.The pesticide residues were determined by gas chromatography-triple quadrupole mass spectrometry.Results There were good linear relationships between 50-1000 ng/ml for the pesticide residues and the correlation coefficients were greater than 0.99.At 0.02,0.1,0.2 mg/kg,the average recoveries of 41 pesticides were 60.6%-110.6%,and the relative standards(RSDs)were 1.3%-16.6%(n=6).Conclusion The method is of high sensitivity,accurate,safe,simple and suitable for determination of pesticide residues in milk.