一种气相色谱质谱联用仪测定土壤中灭多威肟的分析方法

An Analytical Method for the Determination of Methomyl Oxime in Soil by Gas Chromatography-Mass Spectrometry

摘要: 采用加压流体萃取-C18柱净化–气相色谱质谱联用仪测器对土壤中灭多威肟进行分析，对加压流体萃取、净化条件和浓缩条件进行优化。确定最优条件为：萃取溶剂为二氯甲烷–丙酮混合溶剂(1+1)、加压流体萃取温度为70℃，压力为12 Mpa、选择了C18柱作为净化柱，8 mL二氯甲烷–丙酮混合溶剂(1+1)洗脱，20℃减压旋蒸作为收集液的浓缩方式。在最优条件下，土壤样品灭多威肟低、高浓度加标回收效率分别为79.4%~83.7%、90.5%~91.5%，相对标准偏差为0.7%~3.1%，方法检出限为1.17 µg/kg。

Abstract: The methomyl oxime in soil was analyzed by pressurized fluid extraction-C18 column purification-gas chromatographymass spectrometry, and the condition of pressurized fluid extraction, cleanup and concentration were optimized. The optimal conditions were determined as follows: the extraction solvent was dichloromethane-acetone mixed solvent (1+1), the extraction temperature of the pressurized fluid was 70˚C, the pressure was 12 Mpa, the C18 column was selected as the purification column, and 8 mL of dichloromethane-Acetone mixed solvent (1+1) was used to elute, and rotary evaporation under reduced pressure at 20˚C was used as the way to concentrate the collected solution. Under the optimal conditions, the recovery efficiencies of methomyl oxime in low and high concentrations of soil samples were 79.4%~83.7% and 90.5%~91.5%, and the relative standard deviations were 0.7%~3.1%. Furthermore the method detection limit was tested as 1.17 µg/kg.