色谱

色谱 ›› 2013, Vol. 31 ›› Issue (12): 1211-1217.DOI: 10.3724/SP.J.1123.2013.07029

• 研究论文 • 上一篇    下一篇

QuEChERS-在线凝胶色谱-气相色谱-质谱法测定大米、黍子和小麦中34种农药残留

阮华1,2, 荣维广2, 马永建2, 吉文亮2, 刘华良2, 宋宁慧3   

  1. 1. 东南大学公共卫生学院, 江苏 南京 210009;
    2. 江苏省疾病预防控制中心, 江苏 南京 210009;
    3. 环境保护部南京环境科学研究所, 江苏 南京 210042
  • 收稿日期:2013-07-19 修回日期:2013-08-30 出版日期:2013-12-28 发布日期:2013-12-05
  • 通讯作者: 荣维广
  • 基金资助:

    国家自然科学基金项目（41101307）；江苏省“十二·五”科教兴卫工程项目（ZX201109）；江苏省疾病预防控制中心“科教兴业工程”项目（JKRC2011030）

Determination of 34 pesticide residues in rice, proso millet and wheat with QuEChERS-on line gel permeation chromatography-gas chromatography-mass spectrometry

RUAN Hua1,2, RONG Weiguang2, MA Yongjian2, JI Wenliang2, LIU Hualiang2, SONG Ninghui3   

  1. 1. School of Public Health, Southeast University, Nanjing 210009, China;
    2. Jiangsu Center for Disease Prevention and Control, Nanjing 210009, China;
    3. Nanjing Institute of Environment Science, Department of Environmental Protection, Nanjing 210042, China
  • Received:2013-07-19 Revised:2013-08-30 Online:2013-12-28 Published:2013-12-05

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摘要：

采用QuEChERS方法结合在线凝胶色谱-气相色谱-质谱（GPC-GC-MS）系统，建立了大米、黍子和小麦中34种中高毒农药的快速筛查方法。研究了称样量、萃取剂、净化吸附剂种类对大米样品提取净化效果的影响并考察了基质效应和分析保护剂的使用效果，采用选择离子监测（SIM）模式，外标法定量。结果表明，34种农药在大米、黍子和小麦中的检出限分别为0.0281~5.30、0.0282~4.82、0.0273~5.13 μg/kg；在0.05 μg/g添加水平的平均回收率分别为94.5%~117.1%、83.1%~121.7%、93.1%~120.2%；相对标准偏差（RSD，n=6）分别为2.6%~14.5%、3.4%~15.1%、3.5%~15.2%。该方法消耗试剂少，分析成本低，符合绿色化学的理念，具有操作便捷、快速、通用性强等特点，适用于大米、黍子和小麦中34种农药残留的快速筛查与检测。

关键词: QuEChERS, 快速筛查, 凝胶色谱-气相色谱-质谱, 农药残留

Abstract:

A method for the simultaneous determination of 34 pesticides in rice, proso millet and wheat by QuEChERS coupled with on line gel permeation chromatography-gas chromatography-mass spectrometry (GPC-GC-MS) was developed. The effects of the sample weight, extraction solvent, sorbent for purification were investigated. The matrix effect and the usefulness of analyte protectant were also studied. The identification and quantification were performed by GPC-GC-MS in selected ion monitoring (SIM) mode and external standard method. The calibration curves of the 34 pesticides showed good linearity in the range of 0.0125-0.2 mg/L with the correlation coefficients (r2) between 0.968 and 0.999. The average recoveries were 94.5%-117.1%, 83.1%-121.7% and 93.1%-120.2% with the relative standard deviations (RSDs, n=6) no more than 14.5%, 15.1% and 15.2% in rice, proso millet and wheat samples, respectively. The LODs of this method were 0.0281-5.31, 0.0282-4.82 and 0.0273-5.13 μg/kg (S/N=3) for rice, proso millet and wheat samples, respectively. The low cost and less consumption of reagents of this method are in accordance with the concept of green chemistry. The convenient operation and versatility of this method are suitable for the fast screening and detection of the 34 pesticide residues in rice, proso millet and wheat.

Key words: fast screening, gel permeation chromatography-gas chromatography-mass spectrometry (GPC-GC-MS), pesticide residues, QuEChERS

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