气质联用法测定红枣中苯醚甲环唑残留量

Determination of Difenoconazole Residue in Red Jujube by Gas Chromatography-Mass Spectrometry

建立了红枣中苯醚甲环唑残留量的气相色谱–质谱联用(GC–MS)的检测分析方法。样品采用乙腈提取、固相萃取(SPE)柱净化。采用GC–MS分析时,红枣中苯醚甲环唑的3种添加浓度加标回收率在84.4%～93.1%之间,相对标准偏差(RSD)在1.6%～2.8%之间。检出限(LOD,S/N≥3)为0.002 mg/kg,定量下限(LOQ,S/N≥10计)为0.020 mg/kg。在0.05～2.0 mg/L质量浓度范围内呈线性关系,相关系数为0.998 6。该方法可准确用于苯醚甲环唑残留定量分析,方法的灵敏度、精密度和准确度均满足农药残留分析要求。

A residue analytical method was developed for the determination of difenoconazole in red jujube.Difenoconazole residue was extracted with acetonitrile,then purified by a column of SPE,finally concentrated and detected by GC-MS.Its average recoveries were 84.4%-93.1% and its relative standard deviations were 1.6%-2.8%.Its limit of detection（LOD） was 0.002 mg/kg,and its minimum detectable concentration of difenoconazole in the samples was 0.020 mg/kg.The calibration of difenoconazole was linear（correlation coefficient not less than 0.99） within the range of 0.05-2.0 mg/L.The method is suitable for determining difenoconazole residue in red jujube with satisfactory sensitivity,accuracy and precision.