超高效液相色谱-串联质谱法同时测定茶叶中11种植物生长调节剂及吡虫啉、啶虫脒的残留

引用本文: 诸力, 王晨, 陈红平, 张颖彬, 周苏娟, 王国庆, 刘新. 超高效液相色谱-串联质谱法同时测定茶叶中11种植物生长调节剂及吡虫啉、啶虫脒的残留[J]. 分析化学, 2017, 45(4): 529-536. doi: 10.11895/j.issn.0253-3820.160808 shu

Citation: ZHU Li, WANG Chen, CHEN Hong-Ping, ZHANG Ying-Bin, ZHOU Su-Juan, WANG Guo-Qing, LIU Xin. Simultaneous Determination of Plant Growth Regulators and Imidacloprid, Acetamiprid in Tea by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2017, 45(4): 529-536. doi: 10.11895/j.issn.0253-3820.160808 shu

超高效液相色谱-串联质谱法同时测定茶叶中11种植物生长调节剂及吡虫啉、啶虫脒的残留

中国农业科学院茶叶研究所农业部茶叶产品质量安全风险评估实验室(杭州), 杭州 310008
基金项目:
本文系国家茶叶质量安全风险评估重大专项（No.GJFP2016005）、国家茶叶产业技术体系（No.CARS-23）资助

摘要: 建立了超高效液相色谱-串联质谱法同时快速测定茶叶中11种植物生长调节剂（PGRs）及吡虫啉、啶虫脒的方法。样品经乙腈-甲酸溶液（99：1，V/V）均质提取，采用C₁₈、强阴离子交换剂（SAX）、N-丙基乙二胺（PSA）和无水MgSO₄混合吸附剂分散萃取处理，以HSS T3色谱柱分离，采用电喷雾（ESI）正负离子同时扫描和可编程多反应监测模式（SMRM）检测，基质匹配溶液外标法定量。6-苄氨基嘌呤、多效唑、烯效唑、氯吡脲、甲哌啶、吡虫啉、啶虫脒在1~200 μg/L和2，4-二氯苯氧乙酸、对氯苯氧乙酸、赤霉素、吲哚乙酸、萘乙酸、吲哚丁酸在5~1000 μg/L范围内线性良好（R²> 0.99）。13种化合物加标回收率在73.1%~108.9%之间，RSD（n=6）值在0.6%~8.0%之间，方法检出限（LOD，S/N=3）和定量限（LOQ，S/N=10）分别为0.18~9.68 μg/kg和0.61~32.26 μg/kg。本方法简便、稳定、灵敏，能够满足实际检测需求。

关键词:

English

Simultaneous Determination of Plant Growth Regulators and Imidacloprid, Acetamiprid in Tea by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

Laboratory of Quality and Safety Risk Assessment for Tea Ministry of Agriculture, Tea Research Institute, Chinese Academy of Agricultural Sciences, Hangzhou 310008, China
Received Date: 04 November 2016
Revised Date: 20 February 2017

Abstract: An efficient method for the analysis of multiclass plant growth regulators and pesticide (imidacloprid, acetamiprid) residues in tea was developed based on ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted with acetonitrile/formic acid (99:1, V/V) solution, cleaned up with four sorbents including C₁₈, strong anion exchanger (SAX), primary secondary amine (PSA) and anhydrous MgSO₄. The compounds were separated on a HSS T3 column under positive/negative electrospray ionization mode, detected by scheduled multiple reaction monitoring (SMRM), and quantified by matrix-matched external standard curves. All pesticide residues showed good linearity in the concentration range of 1-200 μg/L (6-benzylaminopurine, paclobutrazol, uniconazole, forchlorfenuron, mepiquat chloride, imidacloprid, acetamiprid) or 5-1000 μg/L (2,4-dichlor-ophenoxyacetic acid, 4-chlorophenoxyacetic acid, indole-3-acetic acid, gibberellic acid, 1-naphthaleneacetic acid, indole-3-butyric acid) , with correlation coefficient (R²≥0.99). Limits of detection (LOD, S/N=3) and limits of quantitation (LOQ, S/N=10) were 0.18-9.68 μg/kg and 0.61-32.26 μg/kg, respectively. In addition, the spiked recoveries of tea samples were 73.1%-108.9%, and RSDs were 0.6%-8.0%. This method was applied to commercial samples, and all the detections were confirmed by acquiring transitions for each pesticide in the samples.

Key words:

Tea
/ Plant growth regulator
/ Imidacloprid
/ Acetamiprid
/ Ultra performance liquid chromatography-tandem mass spectrometry
/ Dispersive solid phase extraction

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超高效液相色谱-串联质谱法同时测定茶叶中11种植物生长调节剂及吡虫啉、啶虫脒的残留

English

Simultaneous Determination of Plant Growth Regulators and Imidacloprid, Acetamiprid in Tea by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

超高效液相色谱-串联质谱法同时测定茶叶中11种植物生长调节剂及吡虫啉、啶虫脒的残留

English

Simultaneous Determination of Plant Growth Regulators and Imidacloprid, Acetamiprid in Tea by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

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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通讯作者: 陈斌, bchen63@163.com

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