食品科学 ›› 2011, Vol. 32 ›› Issue (6 ): 159-164.doi: 10.7506/spkx1002-6630-201106036

• 分析检测 • 上一篇    下一篇

气相色谱-质谱法同时测定茶叶中72种农药残留量

陈红平,刘 新,汪庆华,蒋 迎   

  1. 中国农业科学院茶叶研究所,农业部茶叶质量监督检验测试中心
  • 收稿日期:2010-04-16 修回日期:2011-01-07 出版日期:2011-03-25 发布日期:2011-03-03
  • 通讯作者: 陈红平 E-mail:thean27@mail.tricaas.com
  • 基金资助:
    现代农业产业技术体系建设专项(nycytx-26)

Simultaneous Determination of 72 Pesticide Residues in Tea by Gas Chromatography-Mass Spectrometry

CHEN Hong-ping,LIU Xin,WANG Qing-hua,JIANG Ying   

  1. Tea Research Institute, Chinese Academy of Agricultural Sciences, Tea Quality and Supervision Testing Center,
    Ministry of Agriculture, Hangzhou 310008, China
  • Received:2010-04-16 Revised:2011-01-07 Online:2011-03-25 Published:2011-03-03
  • Contact: CHEN Hong-ping E-mail:thean27@mail.tricaas.com

摘要: 建立茶叶中有机氯农药、拟除虫菊酯农药、有机磷农药等72种农药及其异构体多残留的气相色谱-质谱(GC-MS)分析方法。样品加水润湿后,乙腈均质提取,5g/100mL氯化钠溶液与提取液经液液萃取后,再用Carbon/NH2小柱净化,25mL乙酸乙酯-丙酮(1:1)淋洗。优化色谱条件,采用选择离子监测(SIM)模式进行质谱检测。分别在样品中添加标准农药样品0.1、1.0mg/kg水平上进行添加回收率实验,方法的回收率范围为65.3%~142.3%,相对标准偏差为3.0%~20.6%(n=6)。以信噪比RSN=3计算各农药的最低检出限为0.01~0.08mg/kg范围。该方法结果准确、重现性好,满足茶叶中多种农药残留检测要求。

关键词: 茶, 气相色谱-质谱, 农药多残留, 液液萃取, 固相萃取

Abstract: A gas chromatography-mass spectrometry (GC-MS) method was developed for the simultaneous determination of 72 pesticides and their isomers including organochlorine, pyrethriod, organophosphorus and other pesticides in tea. After moistened by water, the samples were subjected to extraction by acetonetrile, preliminary clean up by 5 g/100 mL sodium chloride, and further purification on carbon/NH2 column through the elution using 25 mL of ethyl acetate-acetone (1:1). The MS detection was performed in the selected ion-monitoring mode under the optimal chromatographic conditions. The recovery rates were determined in samples spiked at 0.1 mg/kg and 1.0 mg/kg. The overall recovery rates were 65.3%-142.3%, with a relative standard deviation (RSD) between 3.0% and 20.6%. The detection limit of this method was 0.01-0.08 mg/kg with a signal/noise ratio of 3. This developed method is characteristics of high sensitivity and accuracy, which is suitable for the simultaneous determination of pesticide residues.

Key words: tea, GC-MS, multiple residues, LLE, SPE

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