色谱

色谱

• 特别策划 • 上一篇    下一篇

固相微萃取-气相色谱法和气相色谱-质谱法测定茶叶中氟虫腈及其代谢物残留

周昱, 徐敦明*, 陈达捷, 张志刚, 郑向华, 方恩华   

  1. 厦门出入境检验检疫局检验检疫技术中心, 福建 厦门 361026
  • 收稿日期:2011-04-18 修回日期:2011-05-30 出版日期:2011-07-28 发布日期:2011-08-19
  • 通讯作者: 徐敦明,博士,高级工程师,研究方向为食品安全. Tel: (0592)3269935
  • 基金资助:

    厦门市科技计划项目(3502Z20092009、3502Z20102012)和国家质检总局科技计划项目(2010IK192).

Determination of fipronil and its metabolites in tea by solid-phase microextraction coupled with gas chromatography and gas chromatography-mass spectrometry

ZHOU Yu, XU Dunming*, CHEN Dajie, ZHANG Zhigang, ZHENG Xianghua, FANG Enhua   

  1. Inspection and Quarantine Technology Center, Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China
  • Received:2011-04-18 Revised:2011-05-30 Online:2011-07-28 Published:2011-08-19

PDF

781

被引次数

66

摘要： 基于固相微萃取-气相色谱(SPME-GC)建立了检测茶叶中氟虫腈及其代谢物(脱亚硫酰基氟虫腈、硫化氟虫腈、氟虫腈砜、酰胺氟虫腈)残留的分析方法。实验中采用85 μm聚丙烯酸酯(PA)萃取头,萃取温度为60 ℃,萃取缓冲体系的pH值为9。当添加水平为2～10 μg/kg时,回收率在71.2%～109.3%之间,相对标准偏差(RSD)在1.2%～7.1%之间。方法的检出限(LOD)和定量限(LOQ)分别在0.3～1.2 μg/kg和1.0～4.0 μg/kg之间。对所建立的方法采用气相色谱-质谱(GC-MS)进行确证,结果令人满意。本方法灵敏度、精密度和LOD均符合残留分析要求,具有快速、灵敏度高的特点,适合于茶叶中氟虫腈及其代谢物残留的痕量分析。

关键词: 残留, 茶叶, 代谢物, 氟虫腈, 固相微萃取, 气相色谱, 气相色谱-质谱

Abstract: An effective multi-residue method for the trace analysis of fipronil and four metabolites (fipronil-desulfinyl, fipronil-sulfide, fipronil-sulfone and fipronil-carboxamide) in tea was developed based on solid-phase microextraction coupled with gas chromatography (SPME-GC). The targets were extracted with a fused-silica fiber coated with 85 μm polyacrylate (PA). The extraction was performed in a pH 9 buffer (containing 0.1 mol/L boracic acid, 0.1 mol/L KCl and 0.1 mol/L NaOH) at 60 ℃ and under 2500 r/min for 30 min. With the concentration range of 2~10 μg/kg, the recoveries ranged from 71.2% to 109.3% and the relative standard deviations (RSDs) were lower than 10% (n=6). The limits of detection (LODs) and limits of quantitation (LOQs) of the studied compounds ranged from 0.3 μg/kg to 1.2 μg/kg and 1.0 μg/kg to 4.0 μg/kg, respectively, with the values well below the residue limits set by Japan, European Union and China. By the proposed method, 1 positive samples of 30 tea samples were found with fipronil and fipronil-sulfone. The identification of the method was done by gas chromatography-mass spectrometry (GC-MS). The method can be applied as a monitoring tool for tea, in the investigation of food to fipronil and its metabolites.

Key words: gas chromatography (GC), gas chromatography-mass spectrometry (GC-MS), metabolites, residue, tea, fipronil, solid-phase microextraction (SPME)