注射器内分散固相萃取-超高效液相色谱-串联质谱法快速测定茶叶中24种农药残留

马佳丽; 王晨; 陈红平; 柴云峰; 诸力; 刘新

doi:10.13305/j.cnki.jts.20210804.001

茶叶科学 >

2021 , Vol. 41 >Issue 5: 717 - 730

DOI: https://doi.org/10.13305/j.cnki.jts.20210804.001

研究报告

注射器内分散固相萃取-超高效液相色谱-串联质谱法快速测定茶叶中24种农药残留

马佳丽 ,
王晨 ,
陈红平 ,
柴云峰 ,
诸力 ,
刘新

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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

马佳丽,女,硕士研究生,主要从事茶叶质量安全研究。

收稿日期: 2021-02-01

修回日期: 2021-03-01

网络出版日期: 2021-10-12

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）、国家农产品质量安全风险评估项目（GJFP2020001）

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Rapid Determination of 24 Pesticide Residues in Tea by in-Syringe Dispersive Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

MA Jiali ,
WANG Chen ,
CHEN Hongping ,
CHAI Yunfeng ,
ZHU Li ,
LIU Xin

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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, China

Received date: 2021-02-01

Revised date: 2021-03-01

Online published: 2021-10-12

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摘要

基于茶叶基质特点,开发了注射器内分散固相萃取快速前处理技术,建立了茶叶中24种农药残留超高效液相色谱-串联质谱检测方法。茶叶样品经乙腈提取,无水MgSO₄盐析,在设计的注射器装置内以N-丙基乙二胺键合硅胶和石墨化炭黑作为分散吸附剂进行净化,超高效液相色谱-串联质谱法进行检测。在3个添加水平（0.01、0.05、0.5βmg·kg^-1）下,红茶和绿茶中24种农药的平均回收率为61.7%~98.8%,相对标准偏差为0.4%~5.5%,准确度和精密度良好。24种农药的红茶和绿茶基质标准工作液线性关系良好,相关系数（R²）均大于0.995,检出限（LOD）和定量限（LOQ）分别为0.05~5.36βμg·kg^-1和0.18~17.86βμg·kg^-1,该方法具有良好的灵敏度。本方法具有简便快捷、所需仪器少、省时等优势,适用于茶叶中多农药残留的定量检测。

关键词： 茶叶; 超高效液相色谱-串联质谱; 农药残留; 注射器内分散固相萃取

本文引用格式

马佳丽 , 王晨 , 陈红平 , 柴云峰 , 诸力 , 刘新 . 注射器内分散固相萃取-超高效液相色谱-串联质谱法快速测定茶叶中24种农药残留[J]. 茶叶科学, 2021 , 41(5) : 717 -730 . DOI: 10.13305/j.cnki.jts.20210804.001

Abstract

Based on the characteristics of tea matrix, a rapid pretreatment technology of in-syringe dispersive solid phase extraction (dSPE) was developed, and an analytical method based on ultra high performance liquid chromatography-tandem mass spectrometry was established for the detection of 24 pesticide residues in tea. Tea samples were extracted using acetonitrile, salted-out with MgSO₄, purified with primary secondary amine and graphitized carbon black as dispersive adsorbents in designed syringe devices, and detected by UPLC-MS/MS. Recoveries of 24 pesticides in black and green teas were 61.7%-98.8% at three spiked levels (0.01βmg·kg^-1, 0.05βmg·kg^-1 and 0.5βmg·kg^-1), which indicated high accuracy with the relative standard deviations of 0.4%-5.5%. The calibration curves of 24 pesticides in black and green teas showed good linearity with correlation coefficients (R²) higher than 0.995. The limits of detection (LOD) and the limits of quantitation (LOQ) were 0.05-5.36βμg·kg^-1 and 0.18-17.86βμg·kg^-1, respectively, which show high sensitivity of this method. Being simple, fast, less instrument required and time-saving, this method is suitable for quantification of multiple pesticide residues in tea.

Key words： tea; ultra high performance liquid chromatography-tandem mass spectrometry; pesticide residues; in-syringe dispersive solid phase extraction

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