基于壳聚糖/氧化石墨烯/硅藻土固相萃取-液相色谱串联质谱测定茶叶中多种农药残留

doi:10.13305/j.cnki.jts.2022.02.004

茶叶科学 ›› 2022, Vol. 42 ›› Issue (2): 249-262.doi: 10.13305/j.cnki.jts.2022.02.004

基于壳聚糖/氧化石墨烯/硅藻土固相萃取-液相色谱串联质谱测定茶叶中多种农药残留

胡高华^1,2,3,4, 曹建荣^1,3,4, 杨蕾文宣^1,2,3,4, 王晨^1,3,4, 周苏娟^1,3,4, 刘新^1,3,4, 鲁成银^1,3,4, 陈红平^1,3,4, 马桂岑^1,3,4,*

1.中国农业科学院茶叶研究所,浙江杭州 310008;
2.中国农业科学院研究生院,北京 100081;
3.农业农村部茶叶质量安全控制重点实验室,浙江杭州 310008;
4.农业农村部茶叶产品质量安全风险评估实验室（杭州）,浙江杭州 310008

收稿日期:2021-12-06 修回日期:2022-01-09 出版日期:2022-04-15 发布日期:2022-04-15
通讯作者: * mgc1314@tricaas.com
作者简介:胡高华，男，硕士研究生，主要从事茶叶质量安全与风险评估的研究
基金资助:
财政部和农业农村部: 国家现代农业产业技术体系（ CARS-19 ）、中国农业科学院创新团队（CAAS-ASTIP-2014-TRICAAS-06）、中国农业科学院农业科技创新工程资助（CAAS- ZDRW202011）

Determination of Multi-pesticide Residues in Tea Based on the Combination of CS/GO/DM SPE Column and UPLC-MS/MS

HU Gaohua^1,2,3,4, CAO Jianrong^1,3,4, YANG-LEI Wenxuan^1,2,3,4, WANG Chen^1,3,4, ZHOU Sujuan^1,3,4, LIU Xin^1,3,4, LU Chengyin^1,3,4, CHEN Hongping^1,3,4, MA Guicen^1,3,4,*

1. Tea Research Institute, Chinese Academy of Agriculture Sciences, Hangzhou 310008, China;
2. Graduate School, Chinese Academy of Agriculture Sciences, Beijing 100081, China;
3. Key Laboratory of Tea Quality and Safety Control, Ministry of Agriculture and Rural Affairs, Hangzhou 310008, China;
4. Laboratory of Quality and Safety Risk Assessment for Tea Products (Hangzhou), Ministry of Agriculture and Rural Affairs, Hangzhou 310008

Received:2021-12-06 Revised:2022-01-09 Online:2022-04-15 Published:2022-04-15

摘要/Abstract

摘要： 利用前期合成的壳聚糖/氧化石墨烯/硅藻土固相萃取柱高效吸附茶叶基质,结合超高效液相色谱串联质谱（UPLC-MS/MS）,建立了茶叶中46种农药残留的分析方法。茶叶样品经乙腈提取,固相萃取柱净化,乙腈淋洗等样品前处理,UPLC-MS/MS分析46种农药残留。结果表明,该新型固相萃取净化柱可以高效吸附去除茶叶基质,大大降低基质效应,绿茶、红茶和乌龙茶中农药的基质效应分别下降了4.7%~66.5%,3.2%~35.5%和4.4%~42.8%。在3个加标水平下,46种农药回收率在61.5%~118%线性良好,相关系数（R²）均大于0.98。所建立方法具有吸附剂用量少、省时、无需基质标准溶液、可以检测不同茶类多农残和定量限低等优点。

关键词: 壳聚糖/氧化石墨烯/硅藻土, 基质净化, 农药残留, 茶叶, 超高效液相色谱串联质谱

Abstract: In this study, the synthesized chitosan/graphene oxide/diatomite (CS/GO/DM) solid phase extraction (SPE) column cartridge was used for the purification of tea matrix. A method for determination of 46 kinds of pesticide residues in tea by using ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. The tea samples were extracted by acetonitrile, purified by CS/GO/DM SPE column, washed by acetonitrile. Then, the target compounds of 46 pesticide residues were analyzed by UPLC-MS/MS. The results show that CS/GO/DM SPE column could efficiently remove tea interference substances, which could greatly reduce the matrix effect of pesticides in green tea, black tea and oolong tea by 4.7%-66.5%, 3.2%-35.5% and 4.4%-42.8%, respectively. The recoveries of 46 kinds of pesticides ranged from 61.5% to 118% at three spiked levels, with good linearity. The correlation coefficients (R²) were all higher than 0.98. The developed method has the great advantages of operation simplicity, time saving, and high cleanup ability with only one kind towards different types of tea, no need for using matrix standard solution and a low amount of adsorbent.

Key words: CS/GO/DM, matrix purification, pesticide residues, tea, UPLC-MS/MS

中图分类号:

胡高华, 曹建荣, 杨蕾文宣, 王晨, 周苏娟, 刘新, 鲁成银, 陈红平, 马桂岑. 基于壳聚糖/氧化石墨烯/硅藻土固相萃取-液相色谱串联质谱测定茶叶中多种农药残留[J]. 茶叶科学, 2022, 42(2): 249-262. doi: 10.13305/j.cnki.jts.2022.02.004.

HU Gaohua, CAO Jianrong, YANG-LEI Wenxuan, WANG Chen, ZHOU Sujuan, LIU Xin, LU Chengyin, CHEN Hongping, MA Guicen. Determination of Multi-pesticide Residues in Tea Based on the Combination of CS/GO/DM SPE Column and UPLC-MS/MS[J]. Journal of Tea Science, 2022, 42(2): 249-262. doi: 10.13305/j.cnki.jts.2022.02.004.

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基于壳聚糖/氧化石墨烯/硅藻土固相萃取-液相色谱串联质谱测定茶叶中多种农药残留

Determination of Multi-pesticide Residues in Tea Based on the Combination of CS/GO/DM SPE Column and UPLC-MS/MS

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