固相萃取-超高效液相色谱串联质谱测定茶产品中吡蚜酮

doi:10.13305/j.cnki.jts.2019.04.009

茶叶科学 ›› 2019, Vol. 39 ›› Issue (4): 440-446.doi: 10.13305/j.cnki.jts.2019.04.009

固相萃取-超高效液相色谱串联质谱测定茶产品中吡蚜酮

余焕^1,2, 周利^1,*, 林琴^1,2, 杨洁^1,2, 孙荷芝¹, 伍旭东³, 王新茹¹, 张新忠¹, 陈宗懋¹, 罗逢健^1,*

1. 中国农业科学院茶叶研究所农产品质量安全研究中心,浙江杭州 310008;
2. 中国农业科学院研究生院,北京 100081;
3. 普洱市质量技术监督综合检测中心,云南普洱 665099

收稿日期:2018-12-13 出版日期:2019-08-15 发布日期:2019-08-19
通讯作者: *lizhou@tricaas.com,lfj@tricaas.com
作者简介:余焕,女,硕士研究生,主要从事农药残留方面的研究,yhteawork@163.com。
基金资助:
国家重点研发计划（2016YFD0200207）、浙江省自然科学基金（LY18C160005）、中国农业科学院创新工程（CAAS-ASTIP-TRICAAS）

Determination of Pymetrozine in Tea Products by Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

YU Huan^1,2, ZHOU Li^1,*, LIN Qin^1,2, YANG Jie^1,2, SUN Hezhi¹, WU Xudong³, WANG Xinru¹, ZHANG Xinzhong¹, CHEN Zongmao¹, LUO Fengjian^1,*

1. Research Center of Quality Safety for Agricultural Products, Tea Research Institute, Chinese Academy of Agricultural Sciences, Hangzhou 310008,China;
2. Graduate School of Chinese Academy of Agricultural Sciences, Beijing 100081, China;
3. Pu'er Comprehensive Technical Testing Center, Pu'er 665099, China

Received:2018-12-13 Online:2019-08-15 Published:2019-08-19

摘要/Abstract

摘要： 建立了Cleanert PCX固相萃取,超高效液相色谱-串联质谱（UPLC-MS/MS）测定干茶、抹茶和速溶茶粉中吡蚜酮残留量的分析方法。干茶、抹茶和速溶茶粉中的吡蚜酮经甲醇和水的混合溶液提取、Cleanert PCX固相萃取柱富集净化和Acquity BEH C₁₈色谱柱分离后,通过UPLC-MS/MS多反应监测模式（MRM）测定,外标法定量。在0.005~1.000 mg·kg^-1添加范围内,吡蚜酮的平均回收率为77.0%~95.1%,相对标准偏差（RSD,n=5）为1.8%~6.9%,方法的定量限（LOQ）为0.005~0.010 mg·kg^-1。该方法在灵敏度、准确度和回收率上均符合农药残留检测的要求,可为茶产品中吡蚜酮残留量的测定和风险评估提供分析方法。

关键词: 吡蚜酮, 茶, 农药残留, 固相萃取法, 高效液相色谱-串联质谱

Abstract: An analytical method for the determination of pymetrozine residues in tea products, including dry tea, matcha and instant tea powder, was established based on Cleanert PCX solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The residual pymetrozine in dry tea, matcha and instant tea powder was extracted by a mixture of methanol and water, cleaned up and concentrated by a Cleanert PCX SPE column, and separated on an Acquity BEH C₁₈ column. Pymetrozine level was detected by UPLC-MS/MS on multiple reaction monitoring (MRM) mode and quantified with external standard method. In the spiked range of 0.005-1.000 mg·kg^-1, the average recovery of pymetrozine was 77.0%-95.1%, and the relative standard deviation (RSD, n=5) ranged from 1.8%-6.9%. The limit of quantitation (LOQ) was 0.005 to 0.010 mg·kg^-1. The sensitivity, precision and recovery of the developed method meet the requirements for residual pesticides analysis in various tea products. The results of this study can provide an analytical method for the determination and risk assessment of pymetrozine in tea products.

Key words: pymetrozine, tea, pesticide residue, solid phase extraction, UPLC-MS/MS

中图分类号:

S571.1
S482

余焕, 周利, 林琴, 杨洁, 孙荷芝, 伍旭东, 王新茹, 张新忠, 陈宗懋, 罗逢健. 固相萃取-超高效液相色谱串联质谱测定茶产品中吡蚜酮[J]. 茶叶科学, 2019, 39(4): 440-446. doi: 10.13305/j.cnki.jts.2019.04.009.

YU Huan, ZHOU Li, LIN Qin, YANG Jie, SUN Hezhi, WU Xudong, WANG Xinru, ZHANG Xinzhong, CHEN Zongmao, LUO Fengjian. Determination of Pymetrozine in Tea Products by Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Journal of Tea Science, 2019, 39(4): 440-446. doi: 10.13305/j.cnki.jts.2019.04.009.

参考文献 20

[1]	Lehotay S J, de Kok A, Hiemstra M. Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection[J]. Journal of AOAC International, 2005, 88(2): 595-614.
[2]	Lehotay S J, Mastovská K, Lightfield A R.Use of buffering and other means to improve results of problematic pesticides in a fast and easy method for residue analysis of fruits and vegetables[J]. Journal of AOAC International, 2005, 88(2): 615-629.
[3]	Komasawa N, Ueki R, Kaminoh Y.Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables[J]. Journal of Chromatography A, 2010, 1217(16): 2548-2560.
[4]	Lee S W, Choi J H, Cho S K, et al.Development of a new QuEChERS method based on dry ice for the determination of 168 pesticides in paprika using tandem mass spectrometry[J]. Journal of Chromatography A, 2011, 1218(28): 4366-4377.
[5]	Hiemstra M, de Kok A. Comprehensive multi-residue method for the target analysis of pesticides in crops using liquid chromatography-tandem mass spectrometry[J]. Journal of Chromatography A, 2007, 1145(1/2): 3-25.
[6]	Gonzálezcurbelo M Á, Lehotay S J, Hernándezborges J, et al.Use of ammonium formate in QuEChERS for high-throughput analysis of pesticides in food by fast, low-pressure gas chromatography and liquid chromatography tandem mass spectrometry[J]. Journal of Chromatography A, 2014, 1358: 75-84.
[7]	Hong J H, Lee C R, Lim J S, et al.Comparison of analytical methods and residue patterns of pymetrozine in aster scaber[J]. Bulletin of Environmental Contamination & Toxicology, 2011, 87(6): 649-652.
[8]	Li C, Yang T, Huangfu W, et al.Residues and dynamics of pymetrozine in rice field ecosystem[J]. Chemosphere, 2011, 82(6): 901-904.
[9]	赵瑞, 李二虎, 李桂红, 等. 高效液相色谱法测定芹菜中的吡蚜酮残留[J]. 农药科学与管理, 2014, 35(9): 33-36.
[10]	单菊菊, 程新胜, 黄兰. 固相萃取-高效液相色谱法测定烟叶中的“吡蚜酮”残留量[J]. 烟草科技, 2010, 49(5): 44-50.
[11]	占绣萍, 黄兰淇, 陈建波, 等. 吡蚜酮在保护地菠菜上的残留量分析及安全使用[J]. 农药科学与管理, 2017, 38(5): 29-34.
[12]	吴绪金, 马婧玮, 刘丹黎, 等. 吡蚜酮在棉叶和土壤中消解动态分析及棉子中残留量膳食摄入评估[J]. 农药, 2017(7): 506-509.
[13]	Al-Rahman S H A, Almaz M M, Ahmed N S. Dissipation of Fungicides, Insecticides, and Acaricide in Tomato Using HPLC-DAD and QuEChERS Methodology[J]. Food Analytical Methods, 2012, 5(3): 564-570.
[14]	王全胜, 曹梦超, 刘雅楠, 等. QuEChERS结合UPLC-ESI-MS/MS分析吡蚜酮和异丙威SC在稻田中的残留特征[J]. 农业环境科学学报, 2015, 34(3): 431-437.
[15]	鲍鏖天, 裴少芬, 唐杏燕, 等. QuEChERS结合高效液相色谱串联质谱快速检测速溶茶粉中八种农药残留[J]. 食品与发酵工业, 2018, 44(5): 232-236.
[16]	张田田, 徐加利, 路兴涛, 等. 吡蚜酮防治茶树假眼小绿叶蝉的效果评价及其残留分析[J]. 山东农业科学, 2015, 47(5): 89-92.
[17]	Zhan X P, Ma L, Huang L Q, et al.The optimization and establishment of QuEChERS-UPLC-MS/MS method for simultaneously detecting various kinds of pesticides residues in fruits and vegetables[J]. Journal of Chromatography B, 2017, 1060: 281-290.
[18]	Hou J B, Xie W, Hong D, et al.Simultaneous determination of ten neonicotinoid insecticides and two metabolites in honey and Royal-jelly by solid-phase extraction and liquid chromatography-tandem mass spectrometry[J]. Food Chemistry, 2019, 270: 204-213.
[19]	周利, 罗逢健, 张新忠, 等. 纳米竹炭分散固相萃取/超高效液相色谱-串联质谱法测定绿茶中的农药多残留[J]. 分析测试学报, 2014, 33(6): 642-647.
[20]	周鹏, 林钦, 黄红霞, 等. 稳定同位素稀释超高效液相色谱-串联质谱法测定饲料中24种禁用兽药含量[J]. 分析化学, 2014, 42(2): 233-238.

固相萃取-超高效液相色谱串联质谱测定茶产品中吡蚜酮

Determination of Pymetrozine in Tea Products by Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

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