Sin-QuEChERS结合超高效液相色谱-高分辨质谱法快速筛查绿茶中农药及代谢物残留

引用本文: 黄合田, 谢双, 涂祥婷, 杨鸿波, 郭峰, 孙晓红, 段亚玲, 李占彬. Sin-QuEChERS结合超高效液相色谱-高分辨质谱法快速筛查绿茶中农药及代谢物残留[J]. 分析化学, 2020, 48(3): 423-430. doi: 10.19756/j.issn.0253-3820.191503 shu

Citation: HUANG He-Tian, XIE Shuang, TU Xiang-Ting, YANG Hong-Bo, GUO Feng, SUN Xiao-Hong, DUAN Ya-Ling, LI Zhan-Bin. Rapid Screening of Pesticide and Metabolites Residues in Green Tea by Sin-QuEChERS with Ultra Performance Liquid Chromatography-High Resolution Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2020, 48(3): 423-430. doi: 10.19756/j.issn.0253-3820.191503 shu

Sin-QuEChERS结合超高效液相色谱-高分辨质谱法快速筛查绿茶中农药及代谢物残留

1.
贵州医科大学公共卫生学院, 环境污染与疾病监控教育部重点实验室, 贵阳 550025;
2.
国家地质实验测试中心, 自然资源部生态地球化学重点实验室, 北京 100037;
3.
贵州省分析测试研究院, 贵阳 550016
基金项目:
本文系国家国际科技合作专项（No.2015DFA41280）、国家自然科学基金项目（No.201966011）、黔科合支撑项目（No.[2016]2578）和中央级公益性科研院所基本科研业务费项目（No.CSJ201906）资助

摘要: 建立了Sin-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非靶向筛查绿茶中农药残留的分析方法。以38种农药及代谢物为质控化合物，优化了分析方法。样品经0.1%甲酸-乙腈溶液提取/盐析、振荡并离心，经Sin-QuEChERS Nano净化柱单步净化，以Thermo Accucore aQ色谱柱（150 mm×2.1 mm，2.6 μm）进行分离，以甲醇和0.1%甲酸-水（含5 mmol/L甲酸铵）为流动相，梯度洗脱。在正离子模式下，以Full MS/ddMS²扫描模式进行分析，各物质的精确分子量偏差小于3.8×10^-6，38种农药及代谢物在各自的线性范围内线性关系良好（R>0.99）。在0.01、0.020和0.05 mg/kg加标水平下，除乙硫甲威和蝇毒磷，各物质的平均回收率为68%-115%，相对标准偏差（RSD）为0.4%-18.9%，定量限（LOQ）为0.005-0.02 mg/kg。采用本方法非靶向快速筛查绿茶样品的残留农药，并定量分析残留水平，共检出10种残留农药。本方法处理过程简便、快速、高效、准确，可用于绿茶中多种农药残留及代谢物的快速筛查。

关键词:

English

Rapid Screening of Pesticide and Metabolites Residues in Green Tea by Sin-QuEChERS with Ultra Performance Liquid Chromatography-High Resolution Mass Spectrometry

1.
School of Public Health, the Key Laboratory of Environmental Pollution Monitoring and Disease Control, Ministry of Education, Guizhou Medical University, Guiyang 550025, China;
2.
National Research Center for Geoanalysis, Key Laboratory of Eco-Geochemistry, Ministry of Natural Resources, Beijing 100037, China;
3.
Guizhou Academy of Testing and Analysis, Guiyang 550016, China
Received Date: 15 August 2019
Revised Date: 10 December 2019
Fund Project:
This work was supported by the International S&T Cooperation Program of China (No. 2015DFA41280), the National Natural Science Foundation of China (No. 201966011), the Soft Science Project of Guizhou Provincial Department of Science and Technology in 2016 (No.[2016]2578), and the Central Undertakings Basic Research Expenses Special Funds (No.CSJ 201906).

Abstract: A method for rapid and non-targeted screening of pesticide residues in green tea by Sin-QuEChERS combined with ultra performance liquid chromatography-Q-Exactive Orbitrap mass spectrometry was developed. The method was optimized using 38 pesticides and metabolites as quality control compounds. The samples were extracted with acetonitrile contained 0.1% formic acid, salted out, shaken, centrifuged, and single-step purified by a Sin-QuEChERS Nano purification column. The separation of sample was performed on a Thermo Accucore aQ (2.1 mm×150 mm, 2.6 μm) column. Methanol and 0.1% formic acid water solution (containing 5 mmol/L ammonium formate) were used as the mobile phase for gradient elution. The analysis was performed in Full MS/ddMS2 scan mode in positive ion mode. The exact molecular weight deviation of each substance was less than 3.8×10^-6. The detection result showed that the 38 pesticides and metabolites had good linear relationships within their respective linear ranges (R>0.99). Except for ethiocarb and phosporine, at the spiked levels of 0.01, 0.02 and 0.05 mg/kg, the average recovery of each substance was 68%-115%, of which the RSDs were 0.4%-18.9%, and the limits of quantification (LOQs) were 0.005-0.020 mg/kg. This method was applied to non-target quickly screen residual pesticides in green tea samples and quantify the residual levels, and 10 pesticide residues were detected. The method was simple, fast, efficient and accurate, and could be used for the rapid screening of multi-pesticide residues and metabolites in green tea.

Key words:

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沈阳化工大学材料科学与工程学院沈阳 110142

Sin-QuEChERS结合超高效液相色谱-高分辨质谱法快速筛查绿茶中农药及代谢物残留

English

Rapid Screening of Pesticide and Metabolites Residues in Green Tea by Sin-QuEChERS with Ultra Performance Liquid Chromatography-High Resolution Mass Spectrometry

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

Sin-QuEChERS结合超高效液相色谱-高分辨质谱法快速筛查绿茶中农药及代谢物残留

English

Rapid Screening of Pesticide and Metabolites Residues in Green Tea by Sin-QuEChERS with Ultra Performance Liquid Chromatography-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

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

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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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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