PMID- 30658770 OWN - NLM STAT- MEDLINE DCOM- 20190329 LR - 20190329 IS - 1873-7072 (Electronic) IS - 0308-8146 (Linking) VI - 281 DP - 2019 May 30 TI - Development of precise GC-EI-MS method to determine the residual fipronil and its metabolites in chicken egg. PG - 85-90 LID - S0308-8146(18)32145-9 [pii] LID - 10.1016/j.foodchem.2018.12.041 [doi] AB - Fipronil is a highly toxic insecticide, and fipronil egg scandal greatly threaten people's health. Herein, a precise and reliable method was developed for the determination of fipronil and three metabolites in chicken egg by GC-EI-MS. Sample pretreatment took about 20 min and baseline separation of four analytes were realized within 12 min by GC-MS. Moreover, the limits of detection were 0.2-0.5 ng g(-1) and the limits of quantitation was 0.5-1 ng g(-1) with relative standard deviations (RSDs) lower that 3.32%. Satisfactory recoveries were get in the range of 81.16-103.57% for three levels of spiked samples. Finally, the developed method has been applied for the analysis of egg samples from four sources. Results showed that fipronil and fipronil-sulfone were detected in three samples, while fipronil-desulfinyl and fipronil-sulfide were totally absent. The method showed great promising in quantification of fipronil and its metabolites in food safety affairs. CI - Copyright (c) 2018. Published by Elsevier Ltd. FAU - Li, Xianjiang AU - Li X AD - Food Safety Laboratory, Division of Metrology in Chemistry, National Institute of Metrology, Beijing 100029, China. FAU - Li, Hongmei AU - Li H AD - Food Safety Laboratory, Division of Metrology in Chemistry, National Institute of Metrology, Beijing 100029, China. Electronic address: lihm@nin.ac.cn. FAU - Ma, Wen AU - Ma W AD - Beijing National Laboratory for Molecular Sciences, The Key Laboratory of Bioorganic Chemistry and Molecular Engineering of Ministry of Education, Institute of Analytical Chemistry, College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, China. FAU - Guo, Zhen AU - Guo Z AD - Food Safety Laboratory, Division of Metrology in Chemistry, National Institute of Metrology, Beijing 100029, China. FAU - Li, Xiuqin AU - Li X AD - Food Safety Laboratory, Division of Metrology in Chemistry, National Institute of Metrology, Beijing 100029, China. FAU - Song, Shanjun AU - Song S AD - Food Safety Laboratory, Division of Metrology in Chemistry, National Institute of Metrology, Beijing 100029, China. FAU - Tang, Hua AU - Tang H AD - Food Safety Laboratory, Division of Metrology in Chemistry, National Institute of Metrology, Beijing 100029, China. FAU - Li, Xiaomin AU - Li X AD - Food Safety Laboratory, Division of Metrology in Chemistry, National Institute of Metrology, Beijing 100029, China. FAU - Zhang, Qinghe AU - Zhang Q AD - Food Safety Laboratory, Division of Metrology in Chemistry, National Institute of Metrology, Beijing 100029, China. LA - eng PT - Journal Article DEP - 20181217 PL - England TA - Food Chem JT - Food chemistry JID - 7702639 RN - 0 (Acetonitriles) RN - 0 (Insecticides) RN - 0 (Pyrazoles) RN - 0 (Sulfones) RN - QGH063955F (fipronil) RN - Z072SB282N (acetonitrile) SB - IM MH - Acetonitriles/analysis MH - Eggs/*analysis MH - *Food Analysis MH - Food Contamination/*analysis MH - Gas Chromatography-Mass Spectrometry MH - Insecticides/*analysis MH - Limit of Detection MH - Pyrazoles/*analysis MH - Reproducibility of Results MH - Sulfones/analysis OTO - NOTNLM OT - Fipronil OT - Gas chromatography tandem mass spectrometry OT - Liquid-liquid re-extraction OT - Protein precipitation OT - Solid-phase extraction EDAT- 2019/01/20 06:00 MHDA- 2019/03/30 06:00 CRDT- 2019/01/20 06:00 PHST- 2018/04/28 00:00 [received] PHST- 2018/11/22 00:00 [revised] PHST- 2018/12/09 00:00 [accepted] PHST- 2019/01/20 06:00 [entrez] PHST- 2019/01/20 06:00 [pubmed] PHST- 2019/03/30 06:00 [medline] AID - S0308-8146(18)32145-9 [pii] AID - 10.1016/j.foodchem.2018.12.041 [doi] PST - ppublish SO - Food Chem. 2019 May 30;281:85-90. doi: 10.1016/j.foodchem.2018.12.041. Epub 2018 Dec 17.