色谱

色谱 ›› 2016, Vol. 34 ›› Issue (2): 194-201.DOI: 10.3724/SP.J.1123.2015.07021

• 研究论文 • 上一篇    下一篇

羟基化多壁碳纳米管分散固相萃取-气相色谱-质谱法测定茶叶中21种有机磷农药

荣杰峰, 韦航, 李亦军, 黄伙水, 许美珠   

  1. 泉州出入境检验检疫局, 福建 泉州 362000
  • 收稿日期:2015-07-21 出版日期:2016-02-08 发布日期:2012-09-11
  • 通讯作者: 荣杰峰
  • 基金资助:

    福建检验检疫局科技计划项目(FK2013-26);国家质检总局项目(2015IK035);安溪县科技计划项目(N[2015]0065).

Determination of 21 organophosphorus pesticides in tea by gas chromatography-mass spectrometry coupled with hydroxylated multi-walled carbon nanotubes based on dispersive solid-phase extraction

RONG Jiefeng, WEI Hang, LI Yijun, HUANG Huoshui, XU Meizhu   

  1. Quanzhou Entry-Exit Inspection & Quarantine Bureau, Quanzhou 362000, China
  • Received:2015-07-21 Online:2016-02-08 Published:2012-09-11
  • Supported by:

    Science and Technology Planning Project of Fujian Entry-Exit Inspection and Quarantine Bureau (Grant No. FK2013-26); Project of General Administration of Quality Supervision, Inspection and Quarantine (Grant No. 2015IK035); Science and Technology Planning Project of Anxi County (Grant No. N[2015]0065).

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212

被引次数

13

摘要：

建立了用羟基化多壁碳纳米管(MWCNTs-OH)、N-丙基乙二胺键合固相吸附剂(PSA)和MgSO4作为吸附剂的改进QuEChERS-气相色谱-质谱快速检测茶叶中21种有机磷农药的方法。茶叶中残留的农药经正己烷-丙酮(2 : 1, v/v)混合溶剂提取,以MWCNTs-OH、PSA和MgSO4去除杂质,离心、过滤后经气相色谱-电子轰击源质谱测定,外标法定量。结果表明,目标化合物在0.01~0.50 mg/kg范围内的线性关系良好。空白茶叶样品在低、中、高3个添加水平下的平均回收率为81.5%~109.4%,相对标准偏差(n=5)为2.3%~10.6%,定量限为0.001~0.040 mg/kg。该方法操作简单、快速、灵敏、成本低,能满足茶叶中常见有机磷农药残留的检测要求。

关键词: 茶叶, 分散固相萃取, 气相色谱-质谱, 羟基化多壁碳纳米管, 有机磷农药

Abstract:

A rapid determination method of 21 organophosphorus pesticides in tea was developed by QuEChERS method using modified multi-walled carbon nanotubes (MWCNTs-OH), primary-secondary amine (PSA) and MgSO4 coupled with gas chromatography-mass spectrometry. The pesticide residues in tea were extracted with a hexane-acetone (2 : 1, v/v) mixture, and cleaned up by dispersive solid-phase extraction using MWCNTs-OH and primary-secondary amine (PSA) as the sorbents. After centrifugation and filtration, the target compounds were analyzed by gas chromatography-mass spectrometry and quantified by the external standard method. Under the optimized conditions, good linearities were obtained in the range of 0.01-0.50 mg/kg. The average recoveries were in the range of 81.5%-109.4% at three spiked levels, with relative standard deviations (RSDs, n=5) of 2.3%-10.6%. The limits of quantification were 0.001-0.040 mg/kg. This method is simple, fast, sensitive, cheap, and can meet the requirements of the rapid detection of organophosphorus pesticides in tea.

Key words: dispersive solid-phase extraction (DSPE), gas chromatography-mass spectrometry (GC-MS), hydroxylated multi-walled carbon nanotubes, organophosphorus pesticides, tea

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