PMID- 29372770 OWN - NLM STAT- MEDLINE DCOM- 20181004 LR - 20181004 IS - 1872-2059 (Electronic) IS - 1000-8713 (Linking) VI - 35 IP - 12 DP - 2017 Dec 8 TI - [Rapid screening of fipronil and its metabolites in egg and egg products by solid phase extraction-liquid chromatography-quadrupole time-of-flight mass spectrometry]. PG - 1216-1223 LID - 10.3724/SP.J.1123.2017.09026 [doi] AB - A method for rapid screening of fipronil and its metabolites in egg and egg products was developed by liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (LC-QTOF MS). The samples were extracted by acid-acetonitrile, cleaned up by PRiME HLB SPE. The separation was performed on a Poroshell 120 EC C18 column (150 mmx3 mm, 2.7 mum) with gradient elution using water and acetonitrile as mobile phases. The target compounds were monitored under negative ionization mode with electrospray ionization (ESI) source and two databases of accurate mass and fragment ions were created. The matrix effects in four kinds of egg and egg products were considered and the quantification was carried out by internal standard method. The results demonstrated that the linear ranges were from 0.1 to 5 mug/L with good correlation coefficients (r(2)>0.99). The limits of detection (LODs, S/N>3) and limits of quantitation (LOQs, S/N>10) were 0.2 mug/kg and 1 mug/kg, respectively. The recoveries of fipronil and its metabolites in different matrixes spiked with 1, 2 and 5 mug/kg varied from 82.6%-98.1%, and the relative standard deviations (RSDs) were between 3.8%-9.9% (n=6). The method can effectively correct the ionization suppression. It is sensitive, accurate and suitable for the rapid screening of fipronil, fipronil sulfide, fipronil sulfone and fipronil desulfinyl in egg, egg noodle, cake and mayonnaise. FAU - Guo, Dehua AU - Guo D AD - Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China. FAU - Shi, Yiyin AU - Shi Y AD - Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China. shiyy@shciq.gov.cn. FAU - Li, You AU - Li Y AD - Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China. FAU - Yi, Xionghai AU - Yi X AD - Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China. FAU - Deng, Xiaojun AU - Deng X AD - Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China. FAU - Xiao, Wenqing AU - Xiao W AD - Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China. FAU - Wang, Jian AU - Wang J AD - Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China. FAU - Li, Xiao AU - Li X AD - Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China. FAU - Liu, Han AU - Liu H AD - Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China. FAU - Shen, Weijian AU - Shen W AD - Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China. LA - chi PT - Journal Article PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 RN - 0 (Pyrazoles) RN - KE7T0T1PQ7 (fipronil sulfone) RN - QGH063955F (fipronil) SB - IM MH - Chromatography, Liquid MH - Eggs/*analysis MH - Food Analysis/*methods MH - Limit of Detection MH - Pyrazoles/*analysis MH - Solid Phase Extraction MH - Tandem Mass Spectrometry OTO - NOTNLM OT - egg and egg products OT - fipronil and its metabolites OT - liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOF MS) OT - screening OT - solid phase extraction (SPE) EDAT- 2018/01/27 06:00 MHDA- 2018/10/05 06:00 CRDT- 2018/01/27 06:00 PHST- 2018/01/27 06:00 [entrez] PHST- 2018/01/27 06:00 [pubmed] PHST- 2018/10/05 06:00 [medline] AID - 10.3724/SP.J.1123.2017.09026 [doi] PST - ppublish SO - Se Pu. 2017 Dec 8;35(12):1216-1223. doi: 10.3724/SP.J.1123.2017.09026.