改良QuEChERS/LC-MS/MS联用检测水稻及其土壤中呋虫胺的方法  

Dinotefuran Residue in Paddy Soil,Brown Rice,Rice Hull and Rice Plant Determined by Modified QuEChERS/LC-MS/MS

作　　者：韩昕炜 康頔[1] 张海珍[1] 卢平[1] 胡德禹[1] 

机构地区：[1]贵州大学精细化工研究开发中心绿色农药与农业生物工程国家重点实验室培育基地和教育部绿色农药与生物工程重点实验室,贵州贵阳550025

出　　处：《贵州农业科学》2016年第5期47-50,共4页Guizhou Agricultural Sciences

基　　金：贵州省重大科技专项"贵州省茶叶;蔬菜质量安全评价;检测和可追溯关键技术研究与应用"[黔科合重大专项字(2013)6024];贵州大学创新基金项目"20%呋虫胺泡腾片在水稻上的残留分析及消解动态研究"(2015048)

摘　　要：为了寻求水稻中快速定量检测呋虫胺的方法,稻田土壤、糙米、稻壳及植株样品采用改良的QuEChERS法处理,稻壳和植株样品采用PSA和C18吸附剂净化,LC-MS/MS检测,外标法定量,建立改良QuEChERS/LC-MS/MS联用分析检测水稻田中的呋虫胺。结果表明：在0.015～0.4mg/kg添加水平范围内,稻田土壤、糙米、稻壳以及植株中的平均回收率分别为92.32%～97.45%,93.90%～101.0%,84.30%～99.20%和77.50%～79.00%;相对标准偏差（RSD,n=5）分别为3.52%～4.32%,1.20%～2.60%,0.60%～3.30%和1.20%～2.00%。此方法的最低检测限（LOD）为1.75×10-12 g,最低定量限（LOQ）为5.84×10-12 g。该方法前处理简便,快速,灵敏度高,重现性好,符合农药检测分析的技术要求。The paddy soil,brown rice,rice hull and rice plant samples were first pre-treated with modified QuEChERS,then the rice hull and plant samples were purified by PSA and C18 adsorbent and finally the Dinotefuran residue in four samples was detected by LC-MS/MS to discuss the rapid quantitative method of detecting Dinotefuran residue in paddy soil,brown rice,rice hull and rice plant.Results：The average recovery of paddy soil,brown rice,rice hull and rice plant samples is 92.32% ～97.45%,93.90% ～101.0%,84.30% ～99.20% and 77.50% ～79.00% within the addition range of0.015～0.4mg/kg Dinotefuran separately and RSD of paddy soil,brown rice,rice hull and rice plant samples is 3.52%～4.32%,1.20% ～2.60%,0.60% ～3.30% and 1.20% ～2.00% respectively.The limit of detection（LOD）and limit of quantitation（LOQ）of the modified QuEChERS/LC-MS/MS is1.75×10-12 g and 5.84×10-12 g respectively.The modified QuEChERS/LC-MS/MS with the advantages of simple pretreatment,rapidity,high sensitivity and good repeatability accords with the technical requirement of pesticide detection analysis.

关 键 词：呋虫胺 LC-MS/MS 水稻 残留量 

分 类 号：S482.39[农业科学—农药学]