Residue analysis and persistence evaluation of fipronil and its metabolites in cotton using high-performance liquid chromatography-tandem mass spectrometry.
Residue analysis and persistence evaluation of fipronil and its metabolites in cotton using high-performance liquid chromatography-tandem mass spectrometry.
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DOI：
10.1371/journal.pone.0173690
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发表时间：
2017
期刊：
影响因子：
3.7
通讯作者：
Zheng Y
中科院分区：
文献类型：
--
作者：
Wu X;Yu Y;Xu J;Dong F;Liu X;Du P;Wei D;Zheng Y
建立了一种基于QuEChERS方法和高效液相色谱-串联质谱（UPLC-MS/MS）检测的棉籽、棉株和土壤中氟虫腈及其3种代谢物残留分析方法。在0.005 ~ 0.5 mg/kg水平下，三种基质中四种供试化合物的平均回收率为78.6-108.9%，RSD为0.6 ~ 13.7%。四种供试化合物的定量限（LOQ）范围为0.005 - 0.01 mg/kg。残留动态试验结果表明，氟虫腈在棉株和土壤中的消解速度较快，主要降解途径为氧化和光解。此外，双指数模型表明，氟虫腈在棉花植株和土壤中的测量数据拟合良好，R2在0.8989至0.9989之间。此外，共分析了来自山东省的40个棉籽样品，所有样品均不含四种供试化合物残留。
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.