色谱

色谱 ›› 2018, Vol. 36 ›› Issue (6): 547-551.DOI: 10.3724/SP.J.1123.2017.09043

• 生物基质农兽药残留检测专栏 • 上一篇    下一篇

气相色谱-三重四极杆质谱法快速检测鸡蛋中氟虫腈及其代谢物

邓武剑1, 吴卫东2, 赵旭2, 梁宏2, 梁淑雯2, 靳保辉2, 王申1   

  1. 1. 赛默飞世尔科技(中国)有限公司, 上海 200120;
    2. 深圳出入境检验检疫局, 广东 深圳 518000
  • 收稿日期:2017-09-26 出版日期:2018-06-08 发布日期:2014-04-24
  • 通讯作者: 王申,E-mail:shen.wang@thermofisher.com

Quick determination of fipronil and its metabolites in eggs by gas chromatography-triple quadrupole mass spectrometry

DENG Wujian1, WU Weidong2, ZHAO Xu2, LIANG Hong2, LIANG Shuwen2, JIN Baohui2, WANG Shen1   

  1. 1. Thermo Fisher Scientific(China) Co. Ltd, shanghai 2100120, China;
    2. Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen 518000, China
  • Received:2017-09-26 Online:2018-06-08 Published:2014-04-24

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摘要：

建立了QuEChERS前处理技术结合气相色谱-三重四极杆质谱（GC-MS/MS）分析鸡蛋中氟虫腈及其代谢物的快速检测方法。样品由乙腈提取，然后经150 mg MgSO4脱水和50 mg N-丙基乙二胺（PSA）、50 mg C18净化，采用农药残留专用柱（TR-Pesticide Ⅱ）进行气相色谱分离，以定时反应监测（timed-SRM）模式进行检测，基质曲线外标法定量。结果表明，氟虫腈及其代谢物在1.0~200 μg/L范围内呈良好线性，线性相关系数（R2）均大于0.999，定量限为0.5~1.0 μg/kg；氟虫腈及其代谢物在3个添加水平（2、5和10 μg/kg）下的加标回收率为87.8%~111.5%，相对标准偏差（RSD，n=3）为2.0%~9.2%，该方法能满足欧盟规定的鸡蛋中氟虫腈及其代谢物的残留检测限量要求。

关键词: QuEChERS, 氟虫腈及其代谢物, 鸡蛋, 气相色谱-三重四极杆质谱

Abstract:

A method was established for the simultaneous determination of fipronil and its metabolites in eggs by gas chromatography-tandem mass spectrometry coupled with QuEChERS. Fipronil and its metabolites were extracted from eggs with acetonitrile, and the solution was dehydrated with 150 mg anhydrous magnesium sulfate. The extracts were purified with 50 mg N-propyl ethylenediamine (PSA) and 50 mg C18, and a capillary column pesticide Ⅱ was used. The analytes were detected in timed selected reaction monitoring (timed-SRM) mode, and were quantified using external standard method with matrix correction standard curves. A good linearity in the range of 1.0-200 μg/L with correlation coefficients (R2)>0.999 was observed. The limits of quantification (LOQs) were between 0.5 and 1.0 μg/kg. The recoveries at three spiked levels (2.0, 5.0 and 10.0 μg/kg) were in the range of 87.8% to 111.5% with RSDs between 2.0% and 9.2% (n=3). This new method satisfied the related regulations of the European Union for the determination of fipronil and its metabolites in eggs.

Key words: eggs, fipronil and its metabolites, gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS), QuEChERS

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