QuEChERS-高效液相色谱-串联质谱法分析甘蓝和土壤中的鱼藤酮

Determination of Rotenone in Cabbage and Soil by QuEChERS-HPLC-MS/MS

采用QuEChERS-液相色谱-串联质谱法(QuEChERS and LC-MS/MS)建立了鱼藤酮在甘蓝及土壤中的残留检测方法。样品前处理采用以乙腈作提取剂、PSA(primary sec-ondary amine,N-丙基乙二胺)为分散净化剂的QuEChERS方法,利用高效液相色谱-串联质谱(HPLC-MS/MS)在多反应离子检测模式下进行检测。在甘蓝和土壤中的添加水平为0.002-0.1mg/kg条件下,鱼藤酮在甘蓝中的添加回收率为78.36%～88.16%(相对标准偏差为6.05%～13.38%),在土壤中的添加回收率为77.94%～89.50%(相对标准偏差为4.70%～12.35%)。鱼藤酮在甘蓝和土壤中的最低检测浓度为0.002mg/kg,最小检出量为1.0×10-11g。该方法样品前处理简单、快速,准确度、精密度和灵敏度均符合农药残留检测要求,适用于甘蓝和土壤中鱼藤酮残留的检测。

A method had been developed to determine rotenone residues in cabbage and soil.Rotenone was extracted with acetonitrile,cleaned up with dispersive method on primary secondary amine,and analyzed by HPLC-MS/MS under multiple reaction monitoring mode.When the concentration of rotenone was quantitative from 0.002 to 0.1mg/kg,the average recoveries of rotenone in cabbage were varied from 78.36% to 88.16% with the coefficient of variation of 6.05% to 13.38%,and the average recoveries of rotenone in soil were varied from 77.94% to 89.50% with the coefficient of variation of 4.70% to 12.35%,respectively.The limit of detection of rotenone in cabbage and soil were 0.002mg/kg.The minimum detectable amount was 1.0×1011g.The results showed that the method is simple,rapid,and characterized with acceptable sensitivity and accuracy to meet the requirements of the pesticide residue analysis.This method was applicable to confirm the residues of rotenone in cabbage and soil.