色谱 ›› 2016, Vol. 34 ›› Issue (3): 263-269.DOI: 10.3724/SP.J.1123.2015.10003

• 研究论文 • 上一篇    下一篇

在线净化-液相色谱-串联质谱法测定茶叶中5种烟碱类农药残留

李慧思1, 黄超群2, 蒋沁婷2, 钟莺莺3, 朱晓雨2, 陈笑梅2, 莫为民1   

  1. 1. 浙江工业大学化学工程学院, 浙江 杭州 310014;
    2. 浙江出入境检验检疫局, 浙江 杭州 310016;
    3. 宁波出入境检验检疫局, 浙江 宁波 315012
  • 收稿日期:2015-10-07 出版日期:2016-03-08 发布日期:2012-09-28
  • 通讯作者: 黄超群
  • 基金资助:

    国家质检总局科技计划项目(2015IK302);宁波市重大课题(2007C10035).

Determination of five neonicotinoid pesticide residues in tea by online clean-up-liquid chromatography-tandem mass spectrometry

LI Huisi1, HUANG Chaoqun2, JIANG Qinting2, ZHONG Yingying3, ZHU Xiaoyu2, CHEN Xiaomei2, MO Weimin1   

  1. 1. College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310014, China;
    2. Zhejiang Entry-Exit Inspection and Quarantine Bureau, Hangzhou 310016, China;
    3. Ningbo Entry-Exit Inspection and Quarantine Bureau, Ningbo 315012, China
  • Received:2015-10-07 Online:2016-03-08 Published:2012-09-28
  • Supported by:

    Science and Technology Planning Project of General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China (No. 2015IK302); Major Issue of Ningbo (No. 2007C10035).

摘要:

建立了在线净化-液相色谱-串联质谱测定茶叶中吡虫啉、啶虫脒、噻虫啉、噻虫嗪和噻虫胺5种常见烟碱类农药残留量的方法。样品经水浸泡、乙腈提取和在线净化后,用液相色谱-串联质谱测定。结果表明,本方法对5种烟碱类农药的定量限均为0.01 mg/kg。5种烟碱类农药在1.0~10 μ g/L范围内具有良好的线性关系,相关系数均大于0.998。在0.01、0.02和0.05 mg/kg的添加水平下,回收率为68.0%~113.2%,相对标准偏差为3.2%~7.6%。本方法简便、快速、准确,适用于茶叶样品中烟碱类农药残留量的检测。

关键词: 茶叶, 烟碱类农药, 液相色谱-串联质谱, 在线净化

Abstract:

An online clean-up-liquid chromatography-tandem mass spectrometry method was developed for the determination of five neonicotinoid pesticides (imidacloprid, acetamiprid, thiamethoxam, thiacloprid and clothianidin) in tea. After rehydrated, extracted with acetonitrile, and cleaned-up online, the tea samples were determined by liquid chromatography-tandem mass spectrometry. The results indicated that the limits of quantification for the five neonicotinoid pesticides were 0.01 mg/kg, and the calibration curves were linear in the range of 1.0-10 μ g/L. The spiked recoveries for the five neonicotinoid pesticides from tea were in the range of 68.0%-113.2% with the relative standard deviations between 3.2% and 7.6%. This method is simple, rapid, accurate, and suitable for the simultaneous determination of the five neonicotinoid pesticides in tea.

Key words: liquid chromatography-tandem mass spectrometry (LC-MS/MS), neonicotinoid pesticides, online clean-up, tea

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