色谱 ›› 2018, Vol. 36 ›› Issue (12): 1228-1237.DOI: 10.3724/SP.J.1123.2018.08027

• 研究论文 • 上一篇    下一篇

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

张蓉1,2, 刘鑫1, 彭媛2, 刘韦华1, 张立承1, 代莹1, 李莎莎1, 高志贤2   

  1. 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
  • 收稿日期:2018-08-20 出版日期:2018-12-08 发布日期:2014-11-06
  • 通讯作者: 张蓉,Tel:(010)58619210,E-mail:15301090205@189.cn;高志贤,Tel:(022)8465519l,E-mail:gaozhx@163.com
  • 基金资助:

    国家质量监督检验检疫总局科技计划项目(2016IK027).

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

ZHANG Rong1,2, LIU Xin1, PENG Yuan2, LIU Weihua1, ZHANG Licheng1, DAI Ying1, LI Shasha1, GAO Zhixian2   

  1. 1. Beijing Customs District P. R. China, Beijing 100026, China;
    2. Tianjin Institute of Environmental and Operational Medicine, Tianjin 300050, China
  • Received:2018-08-20 Online:2018-12-08 Published:2014-11-06
  • Supported by:

    General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China (No. 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。

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

Abstract:

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 MS2(Full MS/dd-MS2) 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.

Key words: herbicides, modified QuEChERS, multi-walled carbon nanotubes (MWCNTs), quadrupole/electrostatic field orbitrap high resolution mass spectrometry (Q-Orbitrap HRMS), tea, ultra-high performance liquid chromatography (UHPLC)

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