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:

1. [1]
  Yang C S, Landau J M. J. Nutrition,2000,130(10):2409-2412
2. [2]
  YU Lu, SONG Wei, LU Ya-Ning, ZHAO Mu-Yu, ZHOU Fang-Fang, HU Yan-Yun, ZHENG Ping. Chinese Journal of Chromatography,2015,33(6):597-612 余璐, 宋伟, 吕亚宁, 赵暮雨, 周芳芳, 胡艳云, 郑平.色谱,2015,33(6):597-612
3. [3]
  Huang Z, Zhang Y, Wang L, Ding L, Wang M, Yan H, Li Y, Zhu S. J. Sep. Sci.,2009,32(9):1294-1301
4. [4]
  GB/T 2763-2019, National Food Safety Standard-Maximum Residue Limits of Pesticides in Foods. National Standard of the People's Republic of china.食品安全国家标准-食品中农药最大残留限量.中华人民共和国国家标准. GB/T 2763-2019
5. [5]
  Huang Y, Shi T, Luo X, Hiong H, Min F, Chen Y, Nie S, Xie M. Food Chem.,2019,275:255-264
6. [6]
  Wang J, Chow W, Leung D. J. AOAC Int.,2011,94(6):1685-1714
7. [7]
  Wang S, Liu Y, Jiao S, Zhao Y, Guo Y, Wang M, Zhu G. J. Agr. Food Chem.,2017,65(46):10107-10114
8. [8]
  Chen Q, Hassan M M, Xu J, Zareef M, Li H, Xu Y, Wang P, Agyekum A A, Kutsanedzie F Y H, Viswadevarayalu A. Spectrochim. Acta A,2019,211:86-93
9. [9]
  SU Jian-Feng, ZHONG Mao-Sheng, CHEN Jing, GUO Xi, CHEN Jin-Xing, LIANG Zhen, LIU Jian-Jun. Journal of Instrumental Analysis,2015,34(6):625-638 苏建峰, 钟茂生, 陈晶, 郭昕, 陈劲星, 梁震, 刘建军.分析测试学报,2015,34(6):625-638
10. [10]
  Zhu B, Xu X, Luo J, Jin S, Chen W, Liu Z, Tian C. Food Chem.,2019,276:202-208
11. [11]
  GAO Yi-Xian, CHEN Ping-Hong, NIE Dan-Dan. Chinese Journal of Chromatography,2018,36(6):531-540 高艺羡, 陈萍虹, 聂丹丹.色谱,2018,36(6):531-540
12. [12]
  HUANG Wei, LI Na, XU Rui-Han, LI Ting, LI Chong-Yong. Chinese Journal of Chromatography,2018,36(12):1303-1310 黄微, 李娜, 徐瑞晗, 李婷, 李崇勇.色谱,2018,36(12):1303-1310
13. [13]
  Jiao W, Xiao Y, Qian X, Tong M, Hu Y, Hou R, Hua R. Food Chem.,2016,210:26-34
14. [14]
  Xie W, Han C, Qian Y, Ding H, Chen X, Xi J. Food Chem.,2019,275:255-264
15. [15]
  Saito-Shida S, Hamasaka T, Nemoto S, Akiyama H. Food Chem.,2018,256:140-148
16. [16]
  Dzuman Z, Zachariasova M, Veprikova Z, Godula M, Hajslova J. Anal. Chim. Acta,2015,863:29-40
17. [17]
  WU Ying-Yi, CHEN Zhong, ZHANG Si-Qun, ZHANG Hong. Science and Technology of Food Industry,2019,40(15):188-195 伍颖仪, 陈中, 张思群, 张弘.食品工业科技,2019,40(15):188-195
18. [18]
  Gómez-RamosMaría M D, Rajski L, Horacio H, Fernández-Alba A R. Anal. Bioanal. Chem.,2015,407(21):6317-6326
19. [19]
  Ma G, Zhang M, Zhu L, Chen H, Liu X, Lu C. J. Chromatogr. A,2017,1531:22-31
20. [20]
  CHENG Jing, WANG Mei-Ling, ZHU Shao-Hua, WEN Jiang-Wei, DING Li, WANG Li-Bing. Journal of Food Safety and Quality,2016,7(1):132-137 成婧, 王美玲, 朱绍华, 文江为, 丁利, 王利兵.食品安全质量检测学报,2016,7(1):132-137
21. [21]
  Oellig C, Schwack W. J. Chromatogr. A,2014,1351:1-11
22. [22]
  Wang F, Li S, Feng H, Yang Y, Xiao B, Chen D. Food Chem.,2019,275:530-538
23. [23]
  GAO Yu-Ling, GUO Xiu-Juan, QIAO Shi, SUN Peng. Journal of Tea Science,2017,37(3):243-250 高玉玲, 郭秀娟, 乔石, 孙鹏.茶叶科学,2017,37(3):243-250
24. [24]
  Zhao P, Wang L, Jiang Y, Zhang F, Pan C. J. Agr. Food Chem.,2012,60(16):4026-4033
25. [25]
  Han Y, Song L, Zou N, Chen R, Qin Y, Pan C. J. Chromatogr. B,2016,1031:99-108
26. [26]
  Han Y T, Zou N, Song L, Li Y J, Qin Y H, Liu S W, Li X S, Pan C P. J. Chromatogr.,2015,1005:56-64
27. [27]
  LIU Han, ZHANG Ya-Lian, DING Tao, WANG Sui-Lou, XU Niu-Sheng, GUI Qian-Wen, SHEN Wei-Jian, ZHAO Zeng-Yun, WU Bin, SHEN Chong-Yu, ZHANG Rui. Journal of Instrumental Analysis,2014,33(5):489-498 柳菡, 张亚莲, 丁涛, 王岁楼, 徐牛生, 桂茜雯, 沈伟健, 赵增运, 吴斌, 沈崇钰, 张睿.分析测试学报,2014,33(5):489-498
28. [28]
  WU Bin, DING Tao, LIU Han, CHEN Hui-Lan, ZHAO Zeng-Yun, ZHANG Rui, SHEN Chong-Yu. Chinese Journal of Chromatography,2012,30(12):1246-1252 吴斌, 丁涛, 柳菡, 陈惠兰,赵增运, 张睿, 沈崇钰.色谱,2012, 30(12):1246-1252
29. [29]
  Chen H, Gao G, Chai Y, Ma G, Hao Z, Wang C, Liu X, Lu C. ACS Omega,2017,2(9):5917-5927
30. [30]
  Fan S, Zhao P, Yu C, Pan C, Li X. Food Addit. Contam. A,2014,31(1):73-82
31. [31]
  Song L, Han Y T, Yang J, Qin Y H, Zeng W B, Xu S Q, Pan C P. Food Chem.,2019,279:237-245
32. [32]
  Chen J N, Lian Y J, Zhou Y R, Wang M H, Zhang X Q, Wang J H, Wu Y N, Wang M L. Molecules (Basel, Switzerland),2019,24(16):2918

扫一扫看文章

计量

PDF下载量: 2
文章访问数: 27
HTML全文浏览量: 4

通讯作者: 陈斌, bchen63@163.com

1.
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

计量

文章相关

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处