改进的QuEChERS前处理方法结合超高效液相色谱-串联质谱法同时测定典型叶菜中9种中高风险农药残留  

Determination of 9 pesticide residues in leafy vegetables by modified QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry

作　　者：占绣萍[1] 李建勇[1] 陈建波[1] 马琳[1] 黄兰淇[1] 赵莉[1] ZHAN Xiu-ping;LI Jian-yong;CHEN Jian-bo;MA Lin;HUANG Lan-qi;ZHAO Li(Shanghai Agriculture Technology Extension&Service Centre,Shanghai 201103,China)

机构地区：[1]上海市农业技术推广服务中心,上海201103

出　　处：《农药》2022年第11期833-839,849,共8页Agrochemicals

基　　金：上海市科委科技创新行动计划(19391902300)。

摘　　要：[目的]建立了同时快速检测青菜、生菜、菠菜等典型叶菜中9种常用农药的超高效液相色谱-串联质谱法(UPLC-MS/MS)。[方法]样品采用乙腈溶液直接提取,色素深、基质复杂的叶菜样品采用改进的QuEChERS方法净化,采用电喷雾(ESI)模式电离,多反应监测(MRM)模式检测,基质匹配曲线外标法定量。[结果]该方法在10~500μg/L范围内,具有良好的线性关系,决定系数大于0.99。在10、50、250μg/kg添加质量分数下,平均回收率为71.3%~130.0%,相对标准偏差(RSD)在0.9%~16.0%之间,9种农药方法的定量限为10μg/kg。[结论]该方法简便、快速、灵敏、准确,适于青菜、生菜、菠菜等叶菜中9种农药的残留分析检测要求。经过实际测试,相关9种药剂均未超过国家标准中规定的最大残留限量值。[Aims] This study aims to establish an ultra-high performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method for the determination of 9 pesticide residues in leafy vegetables, including some insecticides and fungicides. [Methods] The leafy vegetable samples were directly extracted with acetonitrile, and purified by modified QuEChERS method. The analysis of 9 pesticides was carried out under electro spray ionization(ESI) mode and multiple reaction monitoring(MRM) mode, quantified by matrix matching curve external standard method.[Results] The results showed that the calibration curves of 9 pesticides were linear(R~2≥0. 99) in the concentration range of 10-500 μg/L. The average recoveries at three spiked levels of 10, 50 and 250 μg/kg were in the ranges of 71.3%-130.0%, with relative standard deviations of 0.9%-16.0%. The quantitation of limit were 10 μg/kg.[Conclusions] The method is simple, rapid, sensitive and accurate, and was suitable for the confirmation and quantitative determination of multiple pesticide residues in leafy vegetables. According to the actual test, none of the nine related pesticide exceeded the maximum residue limit specified in the national standard.

关 键 词：超高效液相色谱-三重四极杆串联质谱 QuEChERS方法 叶类蔬菜 农药 多残留 

分 类 号：TQ450.2[化学工程—农药化工]