QuEChERS-超高效液相色谱-四极杆/静电场轨道阱高分辨质谱测定蔬菜中61种农药残留  

Determination of 61 Pesticide Residues in Vegetables Using QuEChERS-UPLC-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry

作　　者：韩梅[1] 侯雪[1] 邱世婷[1] 焦颖 HAN Mei;HOU Xue;QIU Shi-ting;JIAO Ying(Laboratory of Quality and Safety Risk Assessment for Agricultural Product(Chengdu),Ministry of Agriculture and Rural Affairs,Analytical and Testing Center,Sichuan Academy of Agricultural Sciences,Chengdu 610066,China)

机构地区：[1]四川省农业科学院分析测试中心农业农村部农产品质量安全风险评估实验室(成都),成都610066

出　　处：《农药》2020年第10期743-749,共7页Agrochemicals

基　　金：国家农产品质量安全风险评估项目(GJFP2019009)。

摘　　要：[目的]以QuEChERS为前处理方法,采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-Q-Exactive MS)技术建立了一种快速筛查蔬菜中61种农药残留的测定方法。[方法]蔬菜样品采用1%乙酸乙腈提取,经硫酸镁、乙二胺-N-丙基硅烷化硅胶(PSA)、石墨化碳(GCB)、C18混合净化剂净化,CAPCELL CORE AQ柱分离,在加热电喷雾电离(HESI)源、全扫描及自动触发二级质谱(Full MS/dd-MS2)监测模式下进行检测。[结果]61种目标物在各自范围内线性关系良好,相关系数(r2)均大于0.99,定量限为1~10μg/kg,平均回收率为70.3%~119.7%,相对标准偏差(RSDs)为0.63%~12.09%。[结论]该方法操作简单,快速,灵敏,适用于蔬菜中61种农药残留的定量筛查。[Aims]This study aims to develop a rapid screening method for residue determination of 61 pesticides in vegetables by using QuEChERS-ultra performance liquid chromatography(UPLC)-quadrupole/electrostatic field orbitrap high resolution mass spectrometry.[Methods]The vegetable sample was extracted by acetonitrile containing acetic acid 1%,purified by a mixed sorbent of magnesium sulfate(MgSO4),primary secondary amine(PSA),graphitized carbon black(GCB)and C18,separated on CAPCELL CORE AQ column.The compounds were detected by full scan/data-dependent MS2(Full MS/dd-MS2)via heating electrospray ionization(HESI)source.[Results]The calibration curves were linear with correlation coefficients of 61 pesticides no less than 0.99,the limits of uantitation(LOQ)were in the ranges of 1-10μg/kg,while the recoveries were in the range of 70.3-119.7%,with the elative standard deviations(RSD)between 0.63-12.09%.[Conclusions]The method is simple,fast,sensitive and can be used for the quick screening and quantitative analysis of 61 pesticide residue in vegetables.

关 键 词：QUECHERS 超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-Q-Exactive MS) 蔬菜 农药残留 

分 类 号：TQ450.2[化学工程—农药化工]