食品科学 ›› 2009, Vol. 30 ›› Issue (14): 276-280.doi: 10.7506/spkx1002-6630-200914061

• 分析检测 • 上一篇    下一篇

气相色谱-质谱法测定茶叶中36种农药残留

蒋俊树1,2,赵 彬2,周 莉2   

  1. 1.安徽国家农业标准化与监测中心 2.安徽大学化学化工学院
  • 收稿日期:2009-05-04 修回日期:2008-11-14 出版日期:2009-07-15 发布日期:2010-12-29
  • 通讯作者: 蒋俊树 E-mail:jjs325@163.com
  • 基金资助:

    安徽省科技攻关项目(08010302216);国家标准制修订项目(20068008-T-469)

Simultaneous Determination of 36 Pesticide Residues in Tea by GC-MS

JIANG Jun-shu1,2,ZHAO Bin2,ZHOU Li2   

  1. 1. National Center of Anhui Agricultural Standardization and Supervision, Hefei 230051, China ;
    2. College of Chemistry and Chemical Engineering, Anhui University, Hefei 230039,China
  • Received:2009-05-04 Revised:2008-11-14 Online:2009-07-15 Published:2010-12-29
  • Contact: JIANG Jun-shu1, E-mail:jjs325@163.com

摘要:

建立气相色谱- 质谱(GC-MS)联用技术同时测定茶叶中36 种农药残留方法。茶叶样品用加速溶剂提取(ASE),凝胶渗透色谱(GPC)净化,气相色谱- 质谱法(GC-MS)的选择离子监测(SIM)方式检测,外标法定量。该方法同时测定了茶叶中36 种农药残留,在0.05、0.2、1.0mg/kg 3 个添加水平,平均加标回收率为67.8%~110.2%,相对标准偏差 (RSD)为1.72%~8.89%, 36 种农药的检出限最低为5μg/kg,最高为50μg/kg。该方法快速、灵敏、准确,各项技术指标均满足国内外农药残留检测限量标准要求,能够很好的应用于茶叶中痕量农药的残留测定。

关键词: 气相色谱质谱联用法, 加速溶剂提取(ASE), 凝胶渗透色谱(GPC), 茶叶, 农药残留

Abstract:

A gas chromatography-mass spectrometry (GC-MS) method was developed for the simultaneous detection of 36 pesticide (including 9 kinds of pyrethroid pesticides, 12 kinds of organochlorine pesticides and 15 kinds of organophosphorus pesticides) residues in tea. The method was based on accelerated solvent extraction (ASE) with a mixture of acetonitrile and dichloromethane (1:1, V/V) and gel permeation chromatography (GPC) cleanup followed by GC-MS analysis of the extracts in selected ion monitoring (SIM) mode. The external standard method was adopted for quantitative analyses. At the three spike levels of 0.05, 0.2 and 1.0 mg/kg, mean recoveries for the 36 pesticides were between 67.8% and 110.2% with a relative standard deviation (RSD) ranging from 1.72% to 8.89%. The limits of detection were between 5 μg/kg and 55 μg/kg. This method is rapid, sensitive and accurate and can meet the demands for determining pesticides in tea samples.

Key words: GC-MS, ASE, GPC, tea, pesticide residue

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