改良QuEChERS结合超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速检测茶叶中95种除草剂残留  

Rapid determination of 95 herbicide residues in tea by modified QuEChERS coupled with ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry

作　　者：张蓉 刘鑫 彭媛 刘韦华 张立承 代莹 李莎莎 高志贤 ZHANG Rong;LIU Xin;PENG Yuan;LIU Weihua;LIU Weihua;DAI Ying;LI Shasha;GAO Zhixian(Beijing Customs District P.R.China,Beijing 100026,China;Tianjin Institute of Environmental and Operational Medicine,Tianjin 300050,China)

机构地区：[1]中华人民共和国北京海关,北京100026 [2]天津环境医学与作业医学研究所,天津300050

出　　处：《色谱》2018年第12期1228-1237,共10页Chinese Journal of Chromatography

基　　金：国家质量监督检验检疫总局科技计划项目(2016IK027)~~

摘　　要：基于改良的QuEChERS方法,建立了超高效液相色谱-高分辨质谱同时测定茶叶中95种常见除草剂残留量的定性定量方法。实验以回收率和色素清除效率为指标,通过评估多壁碳纳米管(MWCNTs)、石墨化炭黑(GCB)、N-丙基乙二胺(PSA)和甲苯等在前处理步骤中的影响,优化了经典QuEChERS方法,最终采用含1%(v/v)乙酸的乙腈-甲苯(9∶1,v/v)溶液提取,结合12. 5 mg GCB、12. 5 mg MWCNTs和150 mg PSA混合吸附剂净化的前处理方法。采用Hypersil Gold C18色谱柱分离,在全扫描和自动触发二级质谱(Full MS/dd-MS2)模式下,用四极杆/静电场轨道阱高分辨质谱检测,基质匹配校准曲线定量。结果表明,茶叶中95种除草剂在3个加标水平下的回收率为63. 3%～129. 1%,相对标准偏差(RSD)为0. 7%～15. 2%。该法简便、灵敏、快速、假阳性率低,适用于茶叶等复杂植物基质样品中多种除草剂的定性定量分析。A qualitative and quantitative method was established based on modified QuEChERS for the simultaneous determination of 95 herbicide residues in tea using ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UHPLC-Q-Orbitrap HRMS).The effects of multi-walled carbon nanotubes(MWCNTs),graphitized carbon black(GCB),primary secondary amine(PSA)and toluene on the precondition step were evaluated in terms of matrix-spiked recovery and pigment clean-up effect.Finally,the modified QuEChERS method was applied,which involved sample extraction with an acetonitrile-toluene(9∶1,v/v)mixture containing 1%(v/v)acetic acid,followed by cleaning with 12.5 mg GCB,12.5 mg MWCNTs and 150 mg PSA.The sample extract was separated on a Hypersil Gold C18 column and analyzed in full scan/data-dependent MS 2(Full MS/dd-MS 2)mode.The target herbicides were quantified by using the matrix-matched standard calibration.The three-level spiked recoveries were between 63.3%and 129.1%with the precision of 0.7%-15.2%.This method is easy,sensitive and rapid and can be applicable to the determination of trace herbicide residues in tea and other plant-derived complex matrix samples.

关 键 词：超高效液相色谱 四极杆/静电场轨道阱高分辨质谱 改良QuEChERS 多壁碳纳米管 除草剂 茶叶 

分 类 号：O658[理学—分析化学]