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Multi-Residue Analysis of Fipronil and Its Metabolites in Eggs by SinChERS-Based UHPLC-MS/MS

한국축산식품학회지 2021년 41권 1호 p.59 ~ 70
Han Keguang, Hua Jin, Zhang Qi, Gao Yuanhui, Liu Xiaolin, Cao Jing, Huo Nairui,
소속 상세정보
 ( Han Keguang ) - Shanxi Agricultural University College of Veterinary Medicine
 ( Hua Jin ) - Taiyuan Customs of the People′s Republic of China
 ( Zhang Qi ) - China Southwest University College of Food Science
 ( Gao Yuanhui ) - Taiyuan Customs of the People′s Republic of China
 ( Liu Xiaolin ) - Taiyuan Customs of the People′s Republic of China
 ( Cao Jing ) - Beijing Vocational College of Agriculture
 ( Huo Nairui ) - Shanxi Agricultural University College of Veterinary Medicine

Abstract


A method for simultaneous detection of fipronil (F) and its metabolites fipronil desulfinyl (FD), fipronil sulfide (FS), fipronil sulfone (FSO) in chicken eggs was applied and validated. It includes single-step, cheap, effective, rugged, safe-based method (SinChERS) for sample preparation and ultra high performance liquid chromatography coupled with mass spectrometry (UHPLC-MS/MS) for chemical analysis. Results suggested that formic acid enhanced the recovery of 4 target residues and 1% supplementation to acetonitrile gained higher recoveries than that of 5%. SinChERS integrated extraction and clean-up steps into one, with shorter time (1.5 h) to operate and higher recoveries (97%?100%) than HLB, Envi-Carb-NH2 and quik-easy-cheap-effectiverugged- safe method (QuEChERS), and it consumed the smallest volume of extracting solvent (10 mL) as QuEChERS. Quantitative analyses using external standard method suggested the linear ranges of 4 target compounds were 1?20 μg/L with R2>0.9947. The limit of detection (S/N>3) and quantification (S/N>10) were 0.3 μg/kg and 1 μg/kg. Recoveries ranged from 89.0% to 104.4%, and the relative standard deviations (n=6) at 1, 10, and 20 μg/kg were lower than 6.03%. Thirty batches of domestic eggs (500 g each) were detected by the established SinChERS-based UHPLC-MS/MS and no target residues were detected in all samples. The method developed in this study is a rapid, sensitive, accurate and economic way for multi-residue analysis of fipronil and its metabolites in eggs.

키워드

single-step; cheap; effective; rugged; safe-based method (SinChERS); fipronil; egg; ultra high performance liquid chromatography coupled with mass spectrometry (UHPLC-MS/MS)

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