Rapid determination of fipronil and its metabolite residues in eggs using ultra performance liquid chromatography-tandem mass spectrometry

doi:10.3724/SP.J.1123.2018.03012

Abstract

Abstract:

A method was developed for the rapid simultaneous determination of fipronil and its metabolite residues in eggs using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The egg samples (2 g) with 2 mL water were extracted with 4 mL acetonitrile. After adding 1 g sodium chloride, the mixture was centrifuged at 9000 r/min for 10 min at 4℃. The suspension was diluted and filtered through a 0.22 μm organic membrane. The analytes were separated on a C18 column (100 mm×2.1 mm, 1.7 μm), and detected under the multiple reaction monitoring (MRM) mode with a negative ESI source. The average recoveries of fipronil and its metabolites varied from 77.4% to 112.1%, and the relative standard deviations were between 4.0% and 13.6% at three spiked levels. The limits of detection (LODs) ranged from 0.10 μg/kg to 0.43 μg/kg. The method is simple, effective, and can be applied to real samples.

Key words: eggs, fipronil and its metabolites, matrix effects, QuEChERS, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

CLC Number:

O658

ZHANG Aizhi, LI Xiangjiang, WANG Zhiqiang, ZHANG Shufen, SONG Yue, CAO Lili, CAI Juemei, CHEN Linji. Rapid determination of fipronil and its metabolite residues in eggs using ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(8): 745-751.

References

[1] Rong J F, Wei H, Li Y J, et al. Guangzhou Chemical Industry, 2013, 41(8):16 荣杰峰, 韦航, 李亦军, 等. 广州化工, 2013, 41(8):16
[2] Codex Alimentarius Commossion. Pesticide Residues in Food and Feed. (2016-07-01)[2018-03-12]. http://www.fao.org/fao-who-codexalimentarius/codex-texts/dbs/pestres/pesticide-detail/zh/?p_id=202
[3] Ministry of Health, Labour and Welfare. Positive List System for Agricultural Chemical Residues in Foods. (2006-05-29)[2018-03-12]. http://www.m5.ws001.squarestart.ne.jp/foundation/agrdtl.php?a._inq.=57000
[4] U.S. Environmental Protection Agency. Code of Federal Regulations (40 CFR Part 180) 180.517 Fipronil; Tolerances for Residues. (2013-12-27)[2018-03-12]. https://www.ecfr.gov/cgi-bin/retrieveECFR?gp=1&SID=c1e9b64e91ca7c78f231c766a80d0c4f&ty=HTML&h=L&mc=true&r=SECTION&n=se40.26.180_1517
[5] EU No. 1127/2014
[6] Lin T, Fan J L, Yang D S, et al. Journal of Instrumental Analysis, 2015, 34(12):1360 林涛, 樊建麟, 杨东顺, 等. 分析测试学报, 2015, 34(12):1360
[7] Wu C, Ren H L, Zhao Z Q, et al. Fujian Analysis & Testing, 2016, 25(5):37 吴成, 任海雷, 赵志强, 等. 福建分析测试, 2016, 25(5):37
[8] Zhang M Y, Bian K, Zhou T, et al. J Chromatogr B, 2016, 1014(1):31
[9] Shen W J, Liu H, Zhang R, et al. Chinese Journal of Chromatography, 2017, 35(12):1224 沈伟健, 柳菡, 张睿, 等. 色谱, 2017, 35(12):1224
[10] Guo D H, Shi Y J, Li Y, et al. Chinese Journal of Chromatography, 2017, 35(12):1216 郭德华, 时逸吟, 李优, 等. 色谱, 2017, 35(12):1216
[11] Li J, Zheng X, Wang H Q, et al. Chinese Journal of Chromatography, 2017, 35(12):1211 励炯, 郑锌, 王红青, 等. 色谱, 2017, 35(12):1211
[12] BS EN 15662:2008
[13] Zhou T, Xiao H X, Zhou Z J. Journal of Environmental & Occupational Medicine, 2017, 34(8):745 周彤, 肖红喜, 周志俊. 环境与职业医学, 2017, 34(8):745
[14] Stahnke H, Kialaus S, Kempe G, et a1. Anal Chem, 2012, 84(3):1474
[15] Li H E.[MS Dissertation]. Jinan:Shandong University, 2016 李红娥.[硕士学位论文]. 济南:山东大学, 2016