State Key Laboratory Breeding Base of Green Pesticide and Agricultural Bioengineering, Key Laboratory of Green Pesticide and Agricultural Bioengineering, Ministry of Education, Guizhou University, Guiyang, P. R. China.
J Sep Sci. 2019 Mar;42(6):1210-1221. doi: 10.1002/jssc.201801163. Epub 2019 Jan 30.
A liquid chromatography with tandem mass spectrometry method was developed and validated to simultaneously determine chlorpyrifos, imidacloprid, and imidacloprid metabolites in soil, wheat grain, and wheat straw matrices. Satisfactory linearity (R ≥ 0.9965) of the method was obtained for all analytes. The ranges of limits of detection and limits of quantification for seven analytes in three matrices were 0.17-66.7 and 0.5-200 μg/kg, respectively. Average recoveries were 72.85-81.25% for chlorpyrifos, 78.54-84.70% for imidacloprid, 73.83-81.03% for imidacloprid olefin, 71.47-80.61% for 5-hydroxy imidacloprid, 71.79-81.32% for imidacloprid urea, 70.42-82.20% for imidacloprid nitroguanidine, and 70.91-82.46% for imidacloprid 6-chloronicotinic acid in soil, wheat grain, and wheat straw. The intra- and interday relative standard deviations were less than 8%. The established method was successfully applied for the residual analysis of chlorpyrifos, imidacloprid, and imidacloprid metabolites in actual soil, wheat grain, and wheat straw samples. The results indicated that the established method could be used to detect trace amounts of chlorpyrifos, imidacloprid, and imidacloprid metabolites in wheat and that the method might be able to provide some data on the detection of these seven compounds in other crops.
建立并验证了一种液相色谱-串联质谱法，用于同时测定土壤、小麦籽粒和麦秸中氯吡硫磷、吡虫啉和吡虫啉代谢物。该方法对所有分析物均具有令人满意的线性（R≥0.9965）。在三种基质中，七种分析物的检出限和定量限范围分别为 0.17-66.7 和 0.5-200μg/kg。氯吡硫磷、吡虫啉、吡虫啉烯烃、5-羟基吡虫啉、吡虫啉脲、吡虫啉硝胍和吡虫啉 6-氯烟碱的平均回收率分别为 72.85-81.25%、78.54-84.70%、73.83-81.03%、71.47-80.61%、71.79-81.32%、70.42-82.20%和 70.91-82.46%。在土壤、小麦籽粒和麦秸中，日内和日间相对标准偏差均小于 8%。该方法成功应用于实际土壤、小麦籽粒和麦秸样品中氯吡硫磷、吡虫啉和吡虫啉代谢物的残留分析。结果表明，该方法可用于检测小麦中痕量的氯吡硫磷、吡虫啉和吡虫啉代谢物，该方法可能能够为其他作物中这七种化合物的检测提供一些数据。
