食品科学 ›› 2009, Vol. 30 ›› Issue (14): 191-193.doi: 10.7506/spkx1002-6630-200914037

• 分析检测 • 上一篇    下一篇

顶空固相微萃取-气质联用快速测定草莓中5种有机磷农药

李润岩1,原现瑞2,李 挥3 ,*,张敬轩3,陈 芳4   

  1. 1.河北科技大学化学与制药工程学院 2.河北省分析测试研究中心,河北科技大学 3.河北省食品安全实验室 4.河北九派制药有限公司
  • 收稿日期:2008-11-07 修回日期:2009-01-21 出版日期:2009-07-15 发布日期:2010-12-29
  • 通讯作者: 李挥 E-mail:hbulihui2008@126.com
  • 基金资助:

    河北省科技攻关项目(05547004D-5);河北省科技支撑计划项目(07276709D)

Headspace Solid-phase Microextraction and Gas Chromatography-Mass Spectrometry for the Rapid Detection of 5 Organophosphorus Pesticide Residues in Strawberries

LI Run-yan1,YUAN Xian-rui2,LI Hui3,*,ZHANG Jing-xuan3,CHEN Fang4   

  1. 1. College of Chemical and Pharmaceutical Engineering, Hebei University of Science and Technology, Shijiazhuang 050018, China;
    2. Analytical and Testing Center of Hebei Province, Hebei University of Science and Technology, Shijiazhuang 050018, China;
    3. Hebei Laboratory of Food Safety, Shijiazhuang 050051, China;
    4. Hebei Jiupai Pharmaceutical Co. Ltd., Shijiazhuang 050000, China
  • Received:2008-11-07 Revised:2009-01-21 Online:2009-07-15 Published:2010-12-29
  • Contact: LI Hui3,*, E-mail:hbulihui2008@126.com

摘要:

采用顶空固相微萃取- 气质联用(HS-SPME-GC/MS)技术建立草莓中二嗪农、倍硫磷、杀螟硫磷、乙基对硫磷和乙硫磷5 种有机磷农药的快速测定方法,实验优化了HS-SPME 萃取条件和GC-MS 条件。结果表明:各组分标准曲线方程为:二嗪农y=23.928x+80.891;倍硫磷y=90.368x - 886.061;杀螟硫磷y = 25.992x+123.012;乙基对硫磷y=92.246x - 431.352;乙硫磷y=62.134x+486.49。线性相关系数R 为0.989~0.998,精密度(n = 5)为7.2%~12.7%,方法检出限为5.2~10.7μg/kg,加标回收率为76%~94%。该方法快速、灵敏、准确、试剂用量少,且各项方法学指标符合检测要求,适合作为食品安全监管与检验的标准方法。

关键词: 草莓, 顶空固相微萃取, 气质联用, 有机磷, 快速测定

Abstract:

A headspace solid-phase microextraction (HS-SPME) method in combination with GC-MS was developed for the rapid determination of diazinon, fenitrothion, fenthion, parathion ethyl and ethion in strawberries. The operating conditions of HS-SPME and GC-MS were optimized. A good linear relationship was found to each of the organophosphorus pesticides and the correlation coefficients were in the range of 0.989-0.998. The precision for determining the organophosphorus pesticides by this method (n = 5) varied from 7.2% to 12.7% and the limits of detection were 5.2-10.7 μg/kg. The spike recoveries ranged 76%- 94%. This method demonstrates many advantages including promptness, sensitivity, accuracy and low solvent consumption and therefore is able to meet the demand for determination of pesticide residues.

Key words: strawberry, headspace solid-phase microextraction, gas chromatography-mass spectrometry, organophosphorus, rapid detection

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