Article

Multi-residue Analysis of Fipronil and its Metabolites in Eggs by SinChERS-based UHPLC-MS/MS

Keguang Han, Jin Hua, Qi Zhang, Yuanhui Gao, Xiaolin Liu, Cao Jing, Nairui Huo*
Author Information & Copyright
1College of Veterinary Medicine at Shanxi Agricultural University, Jinzhong 030801, China.
2Taiyuan customs of the People's Republic of China, Taiyuan 030024, China.
3College of Food Science, Southwest University, Chongqing 400715, China, , Chongqing 400715, China.
4 Beijing Vocational College of Agriculture , Beijing 102442, China.
*Corresponding Author: Nairui Huo, E-mail: tgnrhuo@163.com.

© Copyright 2020 Korean Society for Food Science of Animal Resources. This is an Open-Access article distributed under the terms of the Creative Commons Attribution Non-Commercial License (http://creativecommons.org/licenses/by-nc/3.0/) which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.

Received: Jun 08, 2020 ; Revised: Jul 11, 2020 ; Accepted: Aug 25, 2020

Published Online: Sep 03, 2020

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 SinChERS for sample preparation and UHPLC-MS/MS for chemical analysis. Results suggested that formic acid enhanced the recovery of 4 target residues and 1% supplement to acetonitrile gained higher recoveries than 5% formic acid acetonitrile. SinChERS integrates extraction and clean-up steps into one, with shorter time (1.5 h) to operate and higherrecoveries (97%~100%) than HLB, Envi-Carb-NH2 and QuEChERS, and it consumes the smallest volume of extracting solvent (10 mL) as QuEChERS. Quantitative analyses using external standard method showed the linear ranges of 4 target compounds are 1~20 µg/L with R2>0.9947. The limit of detection (S/N>3) and quantification (S/N>10) was 0.3 μg/kg and 1 μg/kg. Recoveries were from 89.0% to 104.4%, and the relative standard deviations (n=6) at 1, 10, 20 μg/kg were lower than 6.03%. To verify the adaptability and practicality of the established SinChERS-based UHPLC-MS/MS, 30 batches of domestic eggs (500 g each batch) were checked and no target residues were detected in all samples. Therefore, 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.

Keywords: SinChERS; fipronil; egg; UHPLC-MS/MS


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