Wu Xiaohu, Yu Yang, Xu Jun, Dong Fengshou, Liu Xingang, Du Pengqiang, Wei Dongmei, Zheng Yongquan
Institute of Plant Protection, Chinese Academy of Agricultural Sciences, State Key Laboratory for Biolog of Plant Diseases and Insect Pests, Haidian District, Beijing, China.
Solid Waste and Chemicals Management Center, Ministry of Environmental Protection, Yuhuinanlu No.1, Chaoyang District, Beijing, Beijing, China.
PLoS One. 2017 Mar 14;12(3):e0173690. doi: 10.1371/journal.pone.0173690. eCollection 2017.
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.
建立了一种基于QuEChERS方法和超高效液相色谱-串联质谱（UPLC-MS/MS）检测的简单残留分析方法，用于分析棉籽、棉花植株和土壤中的氟虫腈及其三种代谢物。在0.005至0.5 mg/kg水平下，三种基质中四种测试化合物的平均回收率为78.6-108.9%，相对标准偏差（RSD）在0.6至13.7%范围内。四种测试化合物的定量限（LOQ）为0.005至0.01 mg/kg。残留动态实验结果表明，氟虫腈在棉花植株和土壤中迅速消散，氧化和光解是主要降解途径。此外，双指数模型对棉花植株和土壤中氟虫腈的实测数据拟合良好，R2在0.8989至0.9989范围内。此外，对山东省的40份棉籽样品进行了分析，所有样品均未检出四种测试化合物残留。
