基于大气压化学电离的GC-MS/MS法测定动物源性食品中8种酰胺类除草剂残留

Determination of Eight Amide Herbicide Residues in Animal-derived Foods by Gas Chromatography-Atmospheric Pressure Chemical Ionization-Tandem Mass Spectrometry

建立基于大气压化学电离的气相色谱-串联质谱法,测定动物源性食品中8种酰胺类除草剂(甲草胺、乙草胺、丙草胺、丁草胺、敌草胺、吡唑草胺、二甲吩草胺、异丙甲草胺)。采用乙腈提取、EMR-Lipid材料净化作为前处理方法,使用乙酸乙酯稀释乙腈净化液代替溶剂转换,大气压化学电离正离子模式多反应监测测定。结果表明,在猪肉、猪肝、鸡蛋、牛奶基质中,8种酰胺类除草剂的平均加标回收率为63.3%~108%,相对标准偏差为2.51%~13.8%,检出限为0.029~1.3μg/kg,定量限为0.095~4.2μg/kg,基质效应为-11%~12%。本方法可有效降低基质效应,简便、高效、准确、灵敏,可用于动物源性食品中8种酰胺类除草剂的快速定量测定。

A gas chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry(GC-APCI-MS/MS)method was established for the determination of the residues of eight amide herbicides(alachlor,acetochlor,propichlor,butachlor,dichlorochlor,pyrazolam,dimethochlor and metolachlor)in animal-derived foods.The sample pretreatment process involved acetonitrile extraction and enhanced matrix removal(EMR)-lipid cleanup,and ethyl acetate was used to dilute the purified acetonitrile extract instead of solvent conversion.The detection was performed with APCI in the positive ion mode using multi-reaction monitoring(MRM).The results showed that the average recoveries of the eight amide herbicides in spiked pork,pig liver,egg and milk matrices were 63.3%–108%,with relative standard deviation(RSD)2.51%–13.8%.The limit of detection(LOD)was 0.029–1.3μg/kg,the limit of quantitation(LOQ)was 0.095–4.2μg/kg,and the matrix effect was−11%–12%.This method can effectively reduce the matrix effect,and is simple,efficient,accurate,sensitive,and suitable for the rapid quantitative determination of the eight amide herbicides in animal-derived foods.