色谱2011，Vol.29Issue(7)：656-661,6.DOI:10.3724/SP.J.1123.2011.00656
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
Determination of fipronil and its metabolites in tea by solid-phase microextraction coupled with gas chromatography and gas chromatography-mass spectrometry
摘要
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 ( SPMEGC ). 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 KCI and 0.1 mol/L NaOH ) at 60℃ and under 2500 r/min for 30 min. With the concentration range of 2 - 10μg/kg, the recoveries ranged from 71.2％ t0 109.3％ and the relative standard deviations ( RSDs ) were lower than l0％ ( n = 6 ). The limits of detection ( LODs ) and limits of quantitation ( LOQs ) of the studied compounds ranged from 0. 3μg/kg t0 1.2μg/kg and 1.0 μg/kg t0 4. 0μg/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.关键词
固相微萃取/气相色谱/气相色谱-质谱/氟虫腈/代谢物/残留/茶叶Key words
solid-phase microextraction ( SPME ) / gas chromatography ( GC ) / gas chromatography-mass spectrometry ( GC-MS )/ fipronil/ metabolites/ residue/ tea分类
化学化工引用本文复制引用
周昱,徐敦明,陈达捷,张志刚,郑向华,方恩华..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[J].色谱,2011,29(7):656-661,6.基金项目
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). （3502Z20092009、3502Z20102012）
