分散固相萃取-超高效液相色谱-串联质谱法快速检测棉花和土壤中氟铃脲的残留

建立了分散固相萃取-超高效液相色谱-串联质谱快速检测棉花和土壤中氟铃脲残留的分析方法。样品采用乙腈提取,N-丙基乙二胺(PSA)净化,超高效液相色谱分离,电喷雾电离、负离子扫描,三重四级杆串联质谱检测以及基质匹配标准品的外标法定量。结果表明,在0.005~0.5 mg/kg 添加水平范围内,氟铃脲的平均添加回收率在71.1% ~110.0%之间,相对标准偏差在2.7% ~8.4%之间。该方法对土壤、棉叶和棉籽3种基质中氟铃脲的检出限 (LOD)分别为0.04,0.12,0.22 μ g/kg,定量限(LOQ)分别为0.14,0.41,0.74 μ g/kg。方法灵敏度高、操作简便、定量准确、测定浓度范围宽,可用于氟铃脲在棉叶、棉籽和土壤中的残留分析。

Simplified method for determination of hexaflumuron residues in cotton and soil using QuEChERS and UPLC-MS/MS

A rapid method for the determination of hexaflumuron residues in cotton and soil was established based on matrix solid-phase dispersion(QuEChERS) and ultraperformance liquid chromatography-mass spectrometry(UPLC-MS/MS).The sample was extracted by acetonitrile and purified on primary secondary amine(PSA).The mass spectrometer was operated with electrospray in the opposite ion mode(ESI-).The target analytes were quantified by external standard method and matrix-matched standard solution used to compensate for matrix effect.Average recoveries of hexaflumuron in soil and corn samples were found in the range of 71.1% -110.0% at three spiking levels from 0.005 mg/kg to 0.5 mg/kg with relative standard deviations of 2.7% -8.4%.Limits of detections(LOD) of hexaflumuron on soil,cotton leaf and cotton seed were 0.04,0.12 and 0.22 μ g/kg, while limits of quantifications(LOQ) were 0.14,0.41 and 0.74 μ g/kg .The method is simple and suitable for the routine and confirmation analysis on cotton leaf,cotton seed and soil.