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作 者:刘晓鹏 刘秋蕊 杜娟 苏毅 LIU Xiaopeng;LIU Qiurui;DU Juan;SU Yi(Inspection and Testing Center of Binzhou,Binzhou 256600,Shandong,China)
出 处:《农药》2025年第2期134-141,共8页Agrochemicals
摘 要:[目的]建立溴虫氟苯双酰胺及其代谢物在白菜和土壤基质中残留的液相色谱-质谱检测方法,研究溴虫氟苯双酰胺及其代谢物在白菜和土壤中的消解动态和最终残留。[方法]白菜和土壤样品经乙腈提取、PSA固相萃取净化剂净化,通过基质标准曲线进行外标法定量,并对白菜和土壤样品中溴虫氟苯双酰胺及其代谢物的残留量进行测定。[结果]建立的QuEChERS-HPLC-MS/MS方法在0.1~100.0μg/L范围内具有良好的线性,添加回收率在76.59%~115.14%之间,相对标准偏差在0.86%~9.18%之间,能够满足白菜和土壤中溴虫氟苯双酰胺的残留检测需求;山东潍坊、山东泰安2地的消解动态试验结果均符合一级动力学方程,其中白菜中溴虫氟苯双酰胺的半衰期分别为0.69、0.83 d,土壤中溴虫氟苯双酰胺的半衰期分别为0.93、1.25 d;最终残留试验结果表明:施药间隔期为7 d的白菜中溴虫氟苯双酰胺母体及其代谢物的残留量之和为0.017~0.050 mg/kg,白菜中溴虫氟苯双酰胺母体的最终残留量为0.016~0.048 mg/kg,低于相关限量标准要求。[结论]溴虫氟苯双酰胺在白菜上降解速度快,施药间隔期7 d采收不会在白菜上存在残留风险,为溴虫氟苯双酰胺在白菜种植中的安全合理使用提供理论依据和技术支持。[Aims]The aim of this study is to establish a liquid chromatography-mass spectrometry detection method for residues of broflanilide and its metabolites in cabbage and soil matrix,and study their dissipation behavior and final residues in cabbage and soil.[Methods]The samples were extracted by acetonitrile,cleaned up by primary secondary amine.The quantitative analysis was carried out by external standard method of matrix matching standard solution,and the residues of broflanilide and its metabolites in cabbage and soil samples were determined.[Results]The QuEChERS-HPLC-MS/MS method had a good linearity in the range of 0.1-100.0μg/L,and the addition recoveries were 76.59%-115.14%,with a relative standard deviation(RSD)of 0.86%-9.18%,meeting the requirements of residue analysis of broflanilide and its metabolites in cabbage and soil.The dissipation behavior test results in Weifang and Tai′an,Shandong,conformed to the first-order kinetic equation.The half-life of broflanilide in cabbage was 0.69 and 0.83 d,while that in soil was 0.93 and 1.25 d.The total residues of broflanilide and its metabolites in cabbage with a 7-day application interval was 0.017-0.050 mg/kg.The final residue of the broflanilide in cabbage was 0.016-0.048 mg/kg.The final residue was lower than the relevant limit in cabbage.[Conclusions]The degradation rate of broflanilide on cabbage is fast,and there is no residual risk when the interval of harvest is 7 d.The application of broflanilide in the cabbage planting process will not cause harmful residues,which provides theoretical basis and technical support for the safe and rational use of broflanilide in the cabbage.
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