Residue analysis and persistence evaluation of fipronil and its metabolites in cotton using high-performance liquid chromatography-tandem mass spectrometry

A simple residue analytical method based on the QuEChERS approach and high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) detection was developed for the analysis of fipronil and its three metabolites in cottonseed, cotton plant and soil. The average recoveries of four test...

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Bibliographic Details
Published in:PloS one 2017-03, Vol.12 (3), p.e0173690-e0173690
Main Authors: Wu, Xiaohu, Yu, Yang, Xu, Jun, Dong, Fengshou, Liu, Xingang, Du, Pengqiang, Wei, Dongmei, Zheng, Yongquan
Format: Article
Language:English
Subjects:
Agriculture
Analysis
Biology and Life Sciences
Chemical properties
Chromatography
Chromatography, High Pressure Liquid - methods
Cotton
Fipronil
Food safety
Gossypium - chemistry
Handbooks
High performance liquid chromatography
Insecticides - analysis
Laboratories
Liquid chromatography
Loam soils
Mass spectrometry
Mass spectroscopy
Metabolites
Methods
Oxidation
Pesticide Residues - analysis
Pesticides
Photolysis
Physical Sciences
Plant diseases
Pyrazoles - analysis
Reproducibility of Results
Saccharum officinarum
Scientific imaging
Soils
Spectroscopy
Sugarcane
Tandem Mass Spectrometry - methods
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Summary:A simple residue analytical method based on the QuEChERS approach and high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) detection was developed for the analysis of fipronil and its three metabolites in cottonseed, cotton plant and soil. The average recoveries of four test compounds from all three matrices were 78.6-108.9% at the level of 0.005 to 0.5 mg/kg, with an RSD in the range of 0.6 to 13.7%. The limit of quantification (LOQ) of the four test compounds ranged from 0.005 to 0.01 mg/kg. The results of the residual dynamics experiments showed that fipronil dissipated rapidly in cotton plants and soil and that oxidation and photolysis were the main degradation pathways. Moreover, the bi-exponential models demonstrated a good fit of the measured data for fipronil in cotton plants and soil, with R2 in the range of 0.8989 to 0.9989. Furthermore, a total of 40 samples of cottonseed from Shandong Province were analyzed, and all of the samples were free from the four test compound residues.
ISSN:1932-6203
1932-6203
DOI:10.1371/journal.pone.0173690