色谱

色谱 ›› 2014, Vol. 32 ›› Issue (6): 635-639.DOI: 10.3724/SP.J.1123.2014.02016

• 技术与应用 • 上一篇    下一篇

多壁碳纳米管滤过型净化柱净化-超高效液相色谱/串联质谱法同时测定生姜中的涕灭威及其代谢物

马立利1, 贾丽1, 周欣燃1, 刘艳1, 范筱京1, 潘灿平2   

  1. 1. 北京市理化分析测试中心, 北京市食品安全分析测试工程技术研究中心, 北京 100089;
    2. 中国农业大学理学院, 北京 100193
  • 收稿日期:2014-02-17 修回日期:2014-04-17 出版日期:2014-06-08 发布日期:2014-05-22
  • 通讯作者: 刘艳
  • 基金资助:

    北京市财政资金项目（PXM2013_178305_000004，PXM2013_178305_000005，PXM2013_178305_000009）.

Analysis of aldicarb and its metabolites in ginger using ultra performance liquid chromatography-tandem mass spectrometry coupled with multiplug filtration clean up with multiwalled carbon nanotubes

MA Lili1, JIA Li1, ZHOU Xinran1, LIU Yan1, FAN Xiaojing1, PAN Canping2   

  1. 1. Beijing Center for Physical and Chemical Analysis, Beijing Engineering Research Center of Food Safety Analysis, Beijing 100089, China;
    2. College of Science, China Agricultural University, Beijing 100193, China
  • Received:2014-02-17 Revised:2014-04-17 Online:2014-06-08 Published:2014-05-22

PDF

359

被引次数

12

摘要：

建立了多壁碳纳米管滤过型净化柱净化-超高效液相色谱/串联质谱联用技术同时测定生姜中涕灭威及其代谢物的分析方法。生姜样品经乙腈提取后，用多壁碳纳米管滤过型净化柱进行2次反复抽提净化，净化液用氮气吹干，用乙腈-水（5：95，v/v）溶解，采用正离子多反应监测（MRM）模式进行分析，外标法定量。结果表明：涕灭威、涕灭威砜及涕灭威亚砜在0.5~200 μg/L浓度范围内呈线性，其相关系数（r2）均大于0.99；在2、20、200 μg/kg添加水平下，回收率为71.4%~89.8%，相对标准偏差范围为0.7%~13.2%；3种目标物的定量限为1.0~2.0 μg/kg。本方法操作简单，灵敏度、准确度和精密度均满足农药多残留检测技术的要求，适用于生姜中涕灭威及其代谢物残留的快速测定。

关键词: 超高效液相色谱/串联质谱, 代谢物, 多壁碳纳米管, 滤过型净化柱, 生姜, 涕灭威

Abstract:

A simple and rapid pretreatment procedure was developed for the simultaneous determination of aldicarb and its metabolites, aldicarb sulfone and aldicarb sulfoxide, in ginger. The samples were extracted with acetonitrile, and then cleaned up with multiplug filtration using multiwalled carbon nanotubes (MWCNTS). The eluate was dried with nitrogen gas at room temperature, and redissolved in an acetonitrile-water (5:95, v/v) mixture, then quantified by ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) operated in positive multiple reaction monitoring (MRM) mode. A linear relationship was achieved in the range of 0.5-200 μg/L for the peak areas to the mass concentrations of the target compounds with the linear correlation coefficients (r2) higher than 0.99. The recoveries at three spiked levels of 2, 20 and 200 μg/kg were in the range from 71.4% to 89.8% with the relative standard deviations (RSDs, n=6) from 0.7% to 13.2% under the selected conditions. The limits of quantification (LOQ, S/N=10) of aldicarb, aldicarb sulfone, and aldicarb sulfoxide in ginger were 1.0, 2.0 and 1.0 μg/kg, respectively. The results demonstrate that the developed method is rapid, cost-effective, and can meet the requirements of the multiple pesticide residue analysis. The method is applicable to determine aldicarb and its metabolites in ginger.

Key words: aldicarb, ginger, metabolites, multiplug filtration clean-up (m-PFC), multiwalled carbon nanotubes (MWCNTS), ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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