摘要
建立玉米、大豆和土壤中氟噻乙草酯残留的液质串联快速分析检测方法。样品中的氟噻乙草酯经乙腈提取,N-丙基乙二胺（PSA）和多壁碳纳米管（MWCNTs）净化,利用超高压液相色谱-串联质谱（UPLC-MS/MS）在多反应监测模式下进行检测。以碎片离子对404.0/274.0定性、离子对404.0/344.0进行外标法定量。仪器在0.001-1.0 mg/kg范围内,具有良好线性关系。在0.001-1.0 mg/kg添加水平范围内,氟噻乙草酯在玉米、大豆和土壤中的平均回收率为95.8%-105.0%,变异系数为3.1%-7.8%。该方法的检出限（LOD）为0.007-0.014μg/kg,定量限为（LOQ）为1.0μg/kg。本方法简便、快速、准确,能满足国内外法规的要求,可用于玉米、大豆和土壤样品中氟噻乙草酯的农药残留确证检测。
A rapid analytical method for determining fluthiacet-methyl residue in maize, soybean and soil was established based on ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. The fluthiacet-methyl from maize, soybean and soil samples, which was extracted by acetonitrile and cleaned up by primary secondary amine （PSA） and multi-walledcarbon nanotubes （MWCNTs）, was determined by ultra performance liquid chromatography-tandem mass spectrometry under multiple reaction monitoring mode, and the qualitative ion pair was 404.0/274.0, the quantitative ion pair was 404.0/344.0. The method had good linear relationship in the concentration range of 0.001~1.0 mg/kg. The average recoveries of fluthiacet-methyl in maize, soybean and soil were in the range of 95.8%~105.0% at spiked levels from 0.001~1 mg/kg, with relative standard deviations of 3.1%~7.8%. The limits of detections （LOD） on maize, soybean and soil was 0.007~0.014 μg/kg, while the limits of quantification （LOQ） was 1 μg/kg. The method is simple, rapid, and accurate, which can meet the requirements of the domestic and international legislation. The method adapts to confirm residues of fluthiacet-methyl pesticides in maize, soybean and soil samples.
出处
《农技服务》
2015年第3期4-6,共3页
AGRICULTURAL TECHNOLOGY SERVICE
基金
贵州省农业科学院专项:黔农科院院专项[2011]022号
