新型介孔材料-QuEChERS-超高效液相色谱-串联质谱法检测茶叶中10种农药残留

引用本文: 杨松, 刘尚可, 张俊杰, 胡佩杰, 曹常鹏, 邹楠. 新型介孔材料-QuEChERS-超高效液相色谱-串联质谱法检测茶叶中10种农药残留[J]. 分析化学, 2021, 49(5): 830-838. doi: 10.19756/j.issn.0253-3820.201656 shu

Citation: YANG Song, LIU Shang-Ke, ZHANG Jun-Jie, HU Pei-Jie, CAO Chang-Peng, ZOU Nan. Detection of 10 Kinds of Pesticide Residues in Tea Based on Novel Mesoporous Materials-QuEChERS-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2021, 49(5): 830-838. doi: 10.19756/j.issn.0253-3820.201656 shu

新型介孔材料-QuEChERS-超高效液相色谱-串联质谱法检测茶叶中10种农药残留

山东农业大学植物保护学院农药毒理与应用技术省级重点实验室, 泰安 271018

通讯作者: 邹楠,E-mail:zounan1226@163.com

基金项目:
国家重点研发计划项目（No.2018YFC1604401）和广西创新驱动发展专项资金项目（No.AA17204043-1）资助。

摘要: 基于QuEChERS法，以自组装的新型介孔材料（SBA-15-C₁₈）为净化剂，结合超高效液相色谱-串联质谱法（UPLC-MS/MS），建立了茶叶基质中10种农药残留的分析方法。在模板剂作用下，采用溶液化学反应法制备了SBA-15；通过十八烷基硅烷偶联剂在SBA-15表面以原位共缩合法制备了SBA-15-C₁₈，采用扫描电镜和红外光谱进行表征。样品以乙腈提取，经SBA-15-C₁₈、纳米氧化锆和多壁碳纳米管组合净化，利用UPLC-MS/MS外标法定量分析。结果表明，SBA-15-C₁₈具有二维通孔结构，粒径大小均一，呈圆柱形弯曲状，平均粒径在240~340 nm之间。茶叶基质中10种农药在0.0025~0.5 mg/L浓度范围内线性关系良好，相关系数（R²）在0.9978~0.9999之间；在0.01、0.1和20 mg/kg添加水平下，10种农药的平均回收率在72%~111%之间，相对标准偏差在1.0%~6.9%之间。茶叶基质中10种农药的检出限为0.1~0.3 μg/kg，定量限为0.2~0.9 μg/kg。将本方法应用于实际茶叶样品的检测，结果显示，所有样品均符合农药最大残留限量标准。本方法具有灵敏度高、通用性强、准确度高、稳定性好、操作简便等优点，适用于茶叶中农药多残留的检测。

关键词:

English

Detection of 10 Kinds of Pesticide Residues in Tea Based on Novel Mesoporous Materials-QuEChERS-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

Provincial Key Laboratory of Pesticide Toxicology & Application Technique, College of Plant Protection, Shandong Agricultural University, Tai'an 271018, China

Corresponding author: ZOU Nan, zounan1226@163.com

Received Date: 06 November 2020
Revised Date: 19 January 2021
Fund Project:
Supported by the National Key R&D Program of China (No.2018YFC1604401) and the Guangxi Special Fund Project (No.AA17204043-1).

Abstract: Based on QuEChERS and with self-synthesized novel mesoporous materials (SBA-15-C₁₈) as a purification agent, a method for determination of 10 kinds of pesticide residues in tea matrix by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. With the action of template, SBA-15 was prepared by solution chemical reaction method, and SBA-15-C₁₈ was then prepared by in-situ co-condensation method on the surface of SBA-15 with octadecyl silane coupling agent. And they were characterized by scanning electron microscopy and infrared spectroscopy. The sample was extracted with acetonitrile, purified by SBA-15-C₁₈, nano-zirconia and multi-wall carbon nanotube tubes, and quantitatively analyzed by external standard method of UPLC-MS/MS. The results showed that SBA-15-C₁₈ had a two-dimensional through-hole structure, uniform particle size and a cylindrical curved shape, with average particle size of 240-340 nm. In the concentration range of 0.0025-0.5 mg/L, the standard solution concentration of 10 kinds of target pesticides in tea matrix showed a good linear relationship with the corresponding chromatographic response value, and the correlation coefficients were between 0.9978 and 0.9999. The average recoveries of the 10 kinds of pesticides at three addition levels of 0.01, 0.1 and 20 mg/kg were between 72% and 111%, and RSDs were 1.0%-6.9%. The limits of detection of 10 kinds of pesticides in tea matrix were 0.1-0.3 μg/kg, and the limits of quantification were 0.2-0.9 μg/kg. The method was applied to monitoring of the samples of the main tea varieties. The method had many advantages such as high sensitivity, strong versatility, high accuracy, good stability and easy operation, and was suitable for detection of pesticide residues in tea.

Key words:

Tea
/ Mesoporous material SBA-15-C₁₈
/ Ultra performance liquid chromatography-tandem mass spectrometry
/ Pesticide residues

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沈阳化工大学材料科学与工程学院沈阳 110142

新型介孔材料-QuEChERS-超高效液相色谱-串联质谱法检测茶叶中10种农药残留

通讯作者: 邹楠,E-mail:zounan1226@163.com

English

Detection of 10 Kinds of Pesticide Residues in Tea Based on Novel Mesoporous Materials-QuEChERS-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

Corresponding author: ZOU Nan, zounan1226@163.com

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

新型介孔材料-QuEChERS-超高效液相色谱-串联质谱法检测茶叶中10种农药残留

通讯作者: 邹楠,E-mail:zounan1226@163.com

English

Detection of 10 Kinds of Pesticide Residues in Tea Based on Novel Mesoporous Materials-QuEChERS-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

Corresponding author: ZOU Nan, zounan1226@163.com

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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