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

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.