噻嗪酮在稻米中残留分析方法研究  

The Analytical Method Study of Buprofezin Residues in Rice

作　　者：黄兰淇[1] 陈秀[1] 张正炜[1] 占绣萍[1] 马琳[1] 

机构地区：[1]上海市农业技术推广服务中心,上海201103

出　　处：《世界农药》2017年第5期50-53,共4页World Pesticide

摘　　要：建立了稻米中噻嗪酮残留量高效液相色谱-串联质谱检测方法。在样品中加入乙腈,匀浆提取,经改进的QuEChERS方法净化后过膜上机。以甲醇和水(含0.1%甲酸)为流动相梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,外标法定量。噻嗪酮在0.01~1.0 mg/L范围内线性关系良好,相关系数(r)≥0.999;糙米中噻嗪酮回收率为89.02%~94.85%,变异系数为4.43%~5.92%;谷壳中噻嗪酮回收率为87.02%~94.35%,变异系数为0.37%~4.16%。最小检出量为2×10^(-11)g,最小检出浓度为0.01 mg/L。该方法操作简单,快速,准确,满足农药残留分析要求。A method was established for the residue determination of buprofezin in rice by liquid chromatography-tandem mass spectrometry （LC-MS/MS）.Buprofezin was extracted by acetonitrile with homogenizedmixing, purified with improved QuEChERS method, filtered through 0.22 -tm of organic membrane and injected into LC-MS/MS. The analyte was separated with the mobile phases of water and methanol （containing 0.1% formic acid）, detected by MS/MS with positive electrospray ionization （ESI＋） in multiple reaction monitoring （MRM） mode, and quantified by external standard method. The correlation coefficient （r） of buprofezin was not lower than 0.999 in the concentration of 0.01-1.0 mg/L. The average recoveries and coefficient of variations were 89.02%-94.85%, 4.43%-5.92% forrice, and 87.02%-94.35%, 0.37%-4.16% for husk of rice. The minimum detectable amount and concentration was 2×10^-11g and 0.01 mg/L. The method is easy, fast and accurate, and meets the requirements of residue analysis of pesticide.

关 键 词：噻嗪酮 稻米 残留 

分 类 号：S481.8[农业科学—农药学]