色谱

色谱

• 研究论文 • 上一篇    下一篇

微型固相萃取柱结合胃袋式大体积进样-气相色谱-质谱法同时快速测定菠菜中的13种有机磷农药残留

李礼1,许秀丽1,2,丁罡斗1,李翔1,张垚1,孙毅之1,何裕建2,仲维科1,陈彦长1,王大宁1

  

  1. 1.Chinese Academy of Inspection and Quarantine, Beijing 100025, China; 2.College of Chemistry and
    Chemical Engineering, Graduate University of Chinese Academy of Sciences, Beijing 100049, China
  • 收稿日期:2007-01-08 修回日期:2007-04-20 出版日期:2007-07-30 发布日期:1985-06-25
  • 通讯作者: 仲维科

Rapid and Simultaneous Determination of Thirteen Organic Phosphorous Pesticide Residues in Spinach Using Gas Chromatography-Mass Spectrometry Coupled with Stomach Large Volume Injection and
Mini Solid Phase Extraction

LI Li1, XU Xiuli1,2, DING Gangdou1, LI Xiang1, ZHANG Yao1, SUN Yizhi1,HE Yujian2, ZHONG Weike1, CHEN Yanzhang1, WANG Daning1   

  1. 1.Chinese Academy of Inspection and Quarantine, Beijing 100025, China; 2.College of Chemistry and
    Chemical Engineering, Graduate University of Chinese Academy of Sciences, Beijing 100049, China
  • Received:2007-01-08 Revised:2007-04-20 Online:2007-07-30 Published:1985-06-25

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摘要：

利用微型固相萃取柱对样品进行前处理,采用胃袋式大体积进样技术结合气相色谱-质谱(GC-MS),建立了菠菜中13种有机磷农药残留的同时快速分析方法。以保留时间和特征离子丰度比定性,以峰面积外标法定量，以3倍信噪比实验值确定方法的检出限(LODs),以10倍信噪比实验值确定方法的定量限(LOQs)。结果表明,除乐果外,其余12种有机磷农药的添加回收率为76.8%～114.0%,相对标准偏差为1.5%～17.6%,LODs为0.5～25 μg/kg。该方法前处理简单快速，分析成本低,分析时间短,灵敏度、准确度和精密度均符合农药多残留检测技术的要求,适用于食品中多种有机磷农药残留的快速灵敏检测。

关键词: 菠菜 , 固相萃取, 气相色谱-质谱, 胃袋式大体积进样, 有机磷农药

Abstract:

A stomach large volume injection-gas chromatography-mass spectrometry (LVI-GC-MS) coupled with mini solid phase extraction (SPE) method for the rapid and simultaneous determination of 13 organic phosphorous pesticide residues in spinach samples is presented. The compounds were identified with their retention times and the abundance ratios of qualifier and target ions. Quantification was calculated based on the extraction of spiking standards in a blank sample. The limit of detection (LOD) was determined by the experimental value of the signal-to-noise ratio of 3∶1, and the limit of quantification (LOQ) was defined at the experimental value of the signal-to-noise ratio of 10∶1. The recoveries obtained ranged from 76.8% to 114.0% with the relative standard deviations between 1.5% and 17.6% except dimethoate. The LODs ranged from 0.5 to 25 μg/kg. This simple, rapid and reliable method has wide applications for the simultaneous determination of multiple pesticide residues in spinach and possibly other species.

Key words: gas chromatography-mass spectrometry （GC-MS）, organic phosphorous pesticide, spinach , stomach large volume injection （LVI）, solid phase extraction （SPE）