PMID- 22097792 OWN - NLM STAT- MEDLINE DCOM- 20120906 LR - 20161018 IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 29 IP - 7 DP - 2011 Jul TI - [Determination of fipronil and its metabolites in tea by solid-phase microextraction coupled with gas chromatography and gas chromatography-mass spectrometry]. PG - 656-61 AB - 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 microm 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 degrees C and under 2500 r/min for 30 min. With the concentration range of 2-10 microg/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 microg/kg to 1.2 microg/kg and 1.0 microg/kg to 4.0 microg/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. FAU - Zhou, Yu AU - Zhou Y AD - Inspection and Quarantine Technology Center, Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China. FAU - Xu, Dunming AU - Xu D FAU - Chen, Dajie AU - Chen D FAU - Zhang, Zhigang AU - Zhang Z FAU - Zheng, Xianghua AU - Zheng X FAU - Fang, Enhua AU - Fang E LA - chi PT - English Abstract PT - Journal Article PT - Research Support, Non-U.S. Gov't PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 RN - 0 (Insecticides) RN - 0 (Pyrazoles) RN - 0 (Tea) RN - QGH063955F (fipronil) SB - IM MH - Chromatography, Gas/*methods MH - Food Contamination/*analysis MH - Gas Chromatography-Mass Spectrometry/*methods MH - Insecticides/analysis/metabolism MH - Pyrazoles/*analysis/metabolism MH - Solid Phase Microextraction/methods MH - Tea/*chemistry EDAT- 2011/11/22 06:00 MHDA- 2012/09/07 06:00 CRDT- 2011/11/22 06:00 PHST- 2011/11/22 06:00 [entrez] PHST- 2011/11/22 06:00 [pubmed] PHST- 2012/09/07 06:00 [medline] PST - ppublish SO - Se Pu. 2011 Jul;29(7):656-61.