固相萃取和气相色谱法测定大米中氟虫腈(锐劲特)残留

建立运用固相萃取技术检测大米中的氟虫腈残留的气相色谱分析方法。样品经过乙腈/丙酮(70/30)抽提,通过硅酸镁(Florisil)固相萃取(SPE)小柱净化,旋转蒸干后用乙腈定容,应用微池电子捕获检测器(μ ECD)检测。样品在10 μ g/kg、15 μ g/kg和30 μ g/kg三个浓度水平添加,回收率为83.18%、 84.49%和88.85%,方法变异系数为1.60%、 1.89%和1.54%。本方法在大米样品中的最低检测定量限为10 μ g/kg

Determination of fipronil residue in rice with solid-phase extraction and gas chromatograph

A method was developed for the determination of fipronil residue in rice with Solid-phase extraction (SPE) combined with gas chromatograph.Residue was extracted from sample with 70/30 acetonitrile / acetone (v/ v) and purified through florisil SPE column.Being diluted to desired volume with acetonitrile after evaporating just to dryness,the residue was analyzed by Gas chromatograph with microcell electron capture detector.Samples were fortified at three spiking levels.At 10μg/kg,15μg/kg and 30μg/kg levels,the respective mean recoveries of fipronil were 83.18%,84.49% and 88.85%,and the relative standard deviations of repeatability were 1.60%,1.89% and 1.54%.The quantitation limits of residue in rice were 10μg/kg.