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

引用本文: 张蓉, 刘鑫, 彭媛, 刘韦华, 张立承, 代莹, 李莎莎, 高志贤. 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[J]. 色谱, 2018, 36(12): 1228-1237. doi: 10.3724/SP.J.1123.2018.08027 shu

Citation: ZHANG Rong, LIU Xin, PENG Yuan, LIU Weihua, ZHANG Licheng, DAI Ying, LI Shasha, GAO Zhixian. 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[J]. Chinese Journal of Chromatography, 2018, 36(12): 1228-1237. doi: 10.3724/SP.J.1123.2018.08027 shu

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.
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
基金项目:
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。

关键词:

English

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

1.
Beijing Customs District P. R. China, Beijing 100026, China;
2.
Tianjin Institute of Environmental and Operational Medicine, Tianjin 300050, China
Received Date: 20 August 2018
Fund Project:
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China (No. 2016IK027).

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:

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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

English

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

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中国化学会秘书处

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

English

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

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

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CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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