Rapid Determination of 88 Pesticide Residues in Tibetan Tea by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with Improved QuEChERS Method

YAN Xiao-xian; TONG Kai-xuan; ZHU Zhe-hui; XIE Yu-jie; WU Xing-qiang; CHANG Qiao-ying; SHI Zhi-hong; FAN Chun-lin; CHEN Hui

doi:10.12452/j.fxcsxb.23121964

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Rapid Determination of 88 Pesticide Residues in Tibetan Tea by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with Improved QuEChERS Method

Scientific Papers | 更新时间：2024-04-18

- Rapid Determination of 88 Pesticide Residues in Tibetan Tea by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with Improved QuEChERS Method
- Journal of Instrumental Analysis Vol. 43, Issue 4, Pages: 590-599(2024)
- 作者机构：
  
  1.中国检验检疫科学研究院，北京 100176
  2.河北大学化学与材料科学学院，河北保定 071002
  3.西藏自治区产品质量监督检验所，西藏拉萨 850000
- 作者简介：
- 基金信息：
- DOI：10.12452/j.fxcsxb.23121964
  CLC： O657.63;TS207.3
- Published：15 April 2024，
  
  Received：19 December 2023，
  
  Revised：19 January 2024，
- 稿件说明：
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严晓贤,仝凯旋,朱浙辉,谢瑜杰,吴兴强,常巧英,石志红,范春林,陈辉.改进QuEChERS方法结合超高效液相色谱-串联质谱法快速测定藏茶中88种农药残留[J].分析测试学报,2024,43(04):590-599.

YAN Xiao-xian,TONG Kai-xuan,ZHU Zhe-hui,XIE Yu-jie,WU Xing-qiang,CHANG Qiao-ying,SHI Zhi-hong,FAN Chun-lin,CHEN Hui.Rapid Determination of 88 Pesticide Residues in Tibetan Tea by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with Improved QuEChERS Method[J].Journal of Instrumental Analysis,2024,43(04):590-599.
严晓贤,仝凯旋,朱浙辉,谢瑜杰,吴兴强,常巧英,石志红,范春林,陈辉.改进QuEChERS方法结合超高效液相色谱-串联质谱法快速测定藏茶中88种农药残留[J].分析测试学报,2024,43(04):590-599. DOI： 10.12452/j.fxcsxb.23121964.

YAN Xiao-xian,TONG Kai-xuan,ZHU Zhe-hui,XIE Yu-jie,WU Xing-qiang,CHANG Qiao-ying,SHI Zhi-hong,FAN Chun-lin,CHEN Hui.Rapid Determination of 88 Pesticide Residues in Tibetan Tea by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Coupled with Improved QuEChERS Method[J].Journal of Instrumental Analysis,2024,43(04):590-599. DOI： 10.12452/j.fxcsxb.23121964.

摘要

建立了藏茶中88种农药残留的改进QuEChERS/超高效液相色谱-串联质谱（QuEChERS/UPLC-MS/MS）检测方法。藏茶样品以1%乙酸乙腈提取和2 g NaCl盐析处理，经交联聚乙烯基吡咯烷酮（PVPP）、十八烷基键合硅胶（C

）、石墨化炭黑（GCB）净化后，以0.01%甲酸水溶液（含2 mmol/L甲酸铵）和0.01%甲酸甲醇为流动相，采用ACQUITY UPLC BEH C

（50 mm×2.1 mm，1.7 μm）色谱柱在15 min内实现分离。在电喷雾正离子模式下，采用多反应监测（MRM）模式检测，基质匹配标准曲线外标法定量。结果表明，藏茶中88种农药在相应质量浓度范围内线性良好（相关系数

≥ 0.999 0），检出限（LOD）和定量下限（LOQ）分别为0.15~3 μg/kg和0.5~10 μg/kg。在1、2、10倍LOQ 3个加标水平下，平均回收率分别为73.2%~108%、73.2 ~109%、72.5%~110%，相对标准偏差（RSD）均不大于12%。将该方法应用于12批实际样品检测，所有样品均检出农药，其中有4批次样品中吡虫啉超限量值。该方法灵敏度高、简便快捷，能够满足藏茶中88种农药的快速检测要求。

Abstract

An improved QuEChERS/ultra performance liquid chromatography-tandem mass spectrometry（QuEChERS/UPLC-MS/MS） analytical method was developed for the determination of 88 pesticide residues in Tibetan tea. Tibetan tea samples were extracted with 1% acetic acid acetonitrile and salted with 2 g NaCl，cleaned up by polyvinylpyrrolidone（PVPP），octadecyl bonded silica gel（C

） and graphitized carbon black（GCB），and then separated with 0.01% formic acid aqueous solution（containing 2 mmol/L ammonium formate） and 0.01% formic acid methanol as the mobile phases. The analytes were separated on an ACQUITY UPLC BEH C

（50 mm×2.1 mm，1.7 μm） column to achieve the separation within 15 min，detected in electrospray positive ionization mode with multiple reaction monitoring（MRM） mode and quantified by matrix matching curve external standard method. The results showed that 88 pesticides in Tibetan tea showed good linear correlations with correlation coefficients（

） not less than 0.999 0 in the corresponding concentration ranges，and the limits of detection（LODs） and limits of quantitation（LOQs） were in the ranges of 0.15-3 μg/kg and 0.5-10 μg/kg，respectively. Average recoveries of the 88 pesticides in Tibetan tea at three spiked levels（1，2，and 10-fold LOQ） were 73.2%-108%，73.2%-109%，72.5%-110%，and the relative standard deviations（RSDs） were not more than 12%. The method was applied to 12 batches of actual samples and pesticides were detected in all samples，among which 4 batches of imidacloprid exceeded the limit value. The method is sensitive，simple and rapid，and could meet the rapid detection requirements of 88 pesticides in Tibetan tea.

关键词

改进QuEChERS藏茶超高效液相色谱-质谱法农药残留

Keywords

improved QuEChERSTibetan teaultra performance liquid chromatography-mass spectrometrypesticide residues

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