Quick Determination of Residues of Fipronil and Its Metabolites in Tea by QuEChERS Coupled with Gas Chromatography-Tandem Mass Spectrometry with Isotope Internal Standard Calibration

被引：1

作者：

Ni Y. ^{[1
]}

Xu X. ^{[2
]}

Huang B. ^{[2
]}

Xu M. ^{[2
]}

Li Z. ^{[3
]}

机构：

[1] College of Education, Zhejiang University of Technology, Hangzhou

[2] Institute of Physical Chemistry and Toxicology, Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou

[3] College of Chemical Engineering, Zhejiang University of Technology, Hangzhou

来源：

Xu, Xiaomin (chemxuxm@163.com); Li, Zuguang (lzg@zjut.edu.cn) | 1600年 / Chinese Chamber of Commerce卷 / 41期

关键词：

Fipronil and its metabolites; Gas chromatography-tandem mass spectrometry; Isotope internal standard; QuEChERS; Tea;

D O I：

10.7506/spkx1002-6630-20190203-018

中图分类号：

学科分类号：

摘要：

Based on the quick, easy, cheap, effective, rugged and safe (QuEChERS) technique, a method for the simultaneous determination of the residues of fipronil and its metabolites in tea was developed by gas chromatography-tandem mass spectrometry (GC-MS/MS). The samples were added with the internal standard of fipronil-13C2,15N2, and then extracted with acetonitrile after water soaking. The extract was dehydrated with sodium chloride (NaCl) and anhydrous magnesium sulfate (MgSO4) and purified by dispersive solid phase extraction with N-propyl ethylenediamine (PSA) and graphite carbon (GCB) sorbents. The analytes were detected by tandem mass spectrometry using multiple reaction monitoring(MRM), and quantified by the internal standard method. A good linearity in the concentration range of 0.4-100 μg/L with correlation coefficients (R2) > 0.995 was observed. The limits of quantification (LOQs) for both fipronil and its metabolites were 1 μg/kg. The recoveries of fipronil and its metabolites at four spiked levels (1, 5, 20 and 200 μg/kg) were in the range of 76.72%-96.53% with relative standard deviations (RSDs, n = 6) between 4.76% and 13.07%. The method was found to be simple, sensitive, accurate and suitable for the rapid quantitative analysis of fipronil and its metabolites in tea. Its sensitivity could meet the requirement for the residual limitation of the EU and Japan. © 2020, China Food Publishing Company. All right reserved.

引用

页码：312 / 317

页数：5

共 17 条

[1] WANG T L, HU J Y, LIU C L, Et al., Simultaneous determination of insecticide fipronil and its metabolites in maize and soil by gas chromatography with electron capture detection, Environmental Monitoring and Assessment, 186, 5, pp. 2767-2774, (2014)
[2] LOURENCO C T, CARVALHO S M, MALASPINA O, Et al., Oral toxicity of fipronil insecticide against the stingless bee Melipona scutellaris (Latreille, 1811), Bulletin of Environmental Contamination and Toxicology, 89, 4, pp. 921-924, (2012)
[3] GUNASEKARA A S, TRUONG T, GOH K S, Et al., Environmental fate and toxicology of fipronil, Journal of Pesticide Science, 32, 3, pp. 189-199, (2007)
[4] DYK M B, LIU Y, CHEN Z S, Et al., Fate and distribution of fipronil on companion animals and in their indoor residences following spot-on flea treatments[J], Journal of Environmental Science and Health Part B:Pesticides Food Contaminants and Agricultural Wastes, 47, 10, pp. 913-924, (2012)
[5] SCHLENK D, HUGGETT D B, ALLGOOD J, Et al., Toxicity of fipronil and its degradation products to Procambarus sp.: field and laboratory studies, Archives of Environmental Contamination and Toxicology, 41, 3, pp. 325-332, (2001)
[6] LU M Y, DU J, ZHOU P X, Et al., Endocrine disrupting potential of fipronil and its metabolite in reporter gene assays, Chemosphere, 120, pp. 246-251, (2015)
[7] CRAVEDI J P, DELOUS G, ZALKO D, Et al., Disposition of fipronil in rats, Chemosphere, 93, 10, pp. 2276-2283, (2013)
[8] 1
[9] Maximum residue limits (MRLs) list of agricultural chemicals in food (2012)
[10] Current MRL values fipronil

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