丙硫菌唑及代谢物硫酮菌唑在土壤中的残留分析方法及消解

Determination and dissipation of prothioconazole and its metabolite prothioconazole-desthio in soil

初步研究了土壤中丙硫菌唑及代谢物硫酮菌唑的残留分析方法及其在北京和安徽两地土壤中的消解情况。样品经乙腈超声提取,盐析后取上清液,经高效液相色谱-紫外检测器（HPLC-UVD）测定,外标法定量。结果表明：在0.05、0.3和1 mg/kg 3个添加水平下,丙硫菌唑和硫酮菌唑的平均回收率在75%-97%之间,相对标准偏差（RSD）在1.0%-7.8%之间,定量限（LOQ）均为0.05 mg/kg,丙硫菌唑在土壤提取液及前处理过程中会部分转化成代谢产物硫酮菌唑。北京和安徽两地喷施到土壤中的丙硫菌唑会迅速转化为代谢物硫酮菌唑,且硫酮菌唑的残留浓度随时间的延长呈现先升高后降低的趋势。

A method for the determination of prothioconazole and its metabolite prothioconazoledesthio in soil was developed.The dissipations in soil in Beijing and Anhui province under field condition were investigated.Samples were extracted with acetonitrile and determined by high performance liquid chromatography coupled with UV-detector（HPLC-UVD）.At fortified levels of0.05,0.3 and 1 mg/kg,recoveries were between 75%-97%,with relative standard deviations（RSDs） of1.0%-7.8%.The limits of quantification（LOQs） were 0.05 mg/kg,for both prothioconazole and prothioconazole-desthio.Prothioconazole partially converted to its metabolite in the soil extractant and in the extraction process.Prothioconazole-desthio was found in soil shortly after the application of prothioconazole,and its concentration increased first and then decreased.