色谱

色谱 ›› 2013, Vol. 31 ›› Issue (9): 885-893.DOI: 10.3724/SP.J.1123.2013.02020

• 研究论文 • 上一篇    下一篇

气相色谱-质谱法测定蔬菜和水果中193种农药的残留量

崔淑华1, 陈慰双2, 钱家亮3, 段浩3, 刘同英3, 张立东3   

  1. 1. 山东出入境检验检疫局食品农产品检测中心, 山东 青岛 266002;
    2. 中国海洋大学环境科学与工程学院, 山东 青岛 266003;
    3. 临沂出入境检验检疫局检验检疫技术中心, 山东 临沂 276034
  • 收稿日期:2013-02-25 修回日期:2013-04-10 出版日期:2013-09-28 发布日期:2013-09-02
  • 通讯作者: 崔淑华
  • 基金资助:

    山东出入境检验检疫科研课题(SK200824).

Determination of 193 pesticide residues in vegetables and fruits by gas chromatography-mass spectrometry

CUI Shuhua1, CHEN Weishuang2, QIAN Jialiang3, DUAN Hao3, LIU Tongying3, ZHANG Lidong3   

  1. 1. Food and Agricultural Products Testing Agency, Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002, China;
    2. College of Environmental Science and Engineering, Ocean University of China, Qingdao 266003, China;
    3. Inspection and Quarantine Technology Center of Linyi Exit-Entry Inspection and Quarantine Bureau, Linyi 276034, China
  • Received:2013-02-25 Revised:2013-04-10 Online:2013-09-28 Published:2013-09-02

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摘要：

在系统优化固相萃取吸附剂填料类型、洗脱溶剂种类及体积的基础上,建立了蔬菜和水果中193种农药残留的气相色谱-质谱(GC-MS)检测方法。样品经乙腈均质提取,C18/PSA固相萃取柱净化,乙腈洗脱,GC-MS选择离子监测(SIM)模式检测,以磷酸三苯酯内标法定量。结果表明,130种农药在10~1000 μg/L、34种农药在20~1000 μg/L、26种农药在50~1000 μg/L、3种农药在100~1000 μg/L范围内线性关系良好,相关系数为0.9967~1.0000,方法检出限(以信噪比为3计)为0.04~8.26 μg/kg,添加回收率为71.6%~117.9%,相对标准偏差为3.0%~11.8%。该方法样品处理简单快速,相比其他多残留分析方法净化效果好,其灵敏度和选择性明显提高,适用于日常检测工作。

关键词: 农药残留, 气相色谱-质谱, 蔬菜, 水果

Abstract:

On the basis of optimization of solid phase extraction adsorbent, eluting solvent types and amounts, a gas chromatography-mass spectrometric method was developed for the determination of 193 pesticide residues in vegetables and fruits. The analytes were extracted from the samples using acetonitrile. The extract was cleaned-up with a C18/PSA solid-phase extractor, eluted by acetonitrile and analyzed by GC-MS under selected ion monitoring (SIM) mode using triphenyl phosphate (TPP) as internal standard. The linear range was from 10 to 1000 μg/L for 130 pesticides, from 20 to 1000 μg/L for 34 pesticides, from 50 to 1000 μg/L for 26 pesticides, from 100 to 1000 μg/L for the other 3 pesticides with the good correlation coefficients (r≥0.9967). The limits of detection were 0.04-8.26 μg/kg. The mean recoveries of the pesticides were 71.6%-117.9%. The relative standard deviations were 3.0%-11.8%. This method is simple, rapid, sensitive and specific. It is appropriate for the simultaneous identification and quantification of the multi-residues in fruits and vegetables.

Key words: fruits, gas chromatography-mass spectrometry (GC-MS), pesticide residues, vegetables

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