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.

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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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