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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。
QuEChERS-LC-MS / MS was used to establish a method for the determination of rotenone residue in cabbage and soil. The samples were pre-treated with QuEChERS method using acetonitrile as extraction solvent and PSA (primary-ondary amine) as dispersing and purifying agent, using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) Multiple reactive ion detection mode for testing. The recoveries of rotenone in cabbage were 78.36% ~ 88.16% (relative standard deviation 6.05% ~ 13.38%) in the cabbage and soil at the level of 0.002-0.1mg / kg, Rates ranged from 77.94% to 89.50% (relative standard deviations from 4.70% to 12.35%). The minimum detection concentration of rotenone in cabbage and soil is 0.002mg / kg, the minimum detectable amount of 1.0 × 10-11g. The method is simple, rapid, accurate, precise and sensitive. The pretreatment of the method is in line with the requirements of pesticide residue detection and is suitable for the detection of rotenone residues in cabbage and soil.