土壤中20种磺酰脲类除草剂的超高效液相色谱-串联质谱测定方法

建立了加速溶剂提取、凝胶渗透色谱法净化-超高效液相色谱/串联质谱快速测定土壤中20种磺酰脲类除草剂的方法。土壤经过冷冻干燥、粉碎过筛,用加速溶剂仪提取(ASE),经凝胶渗透色谱净化(GPC),以超高效液相色谱/串联质谱(UPLC-MS/MS)多级监测模式(MRM)外标法进行定性定量分析。结果表明:土壤中20种磺酰脲类除藻剂的检出限为2～5 ng/kg。对同一环境样品进行了3个不同添加量(1、5、10μg/L)的加标回收实验,平均回收率为65. 7%～106. 1%,相对标准偏差为2. 3%～12. 1%。该方法快速、灵敏、准确,可有效应用于土壤中20种磺酰脲类除草剂的快速监测。

Method for Determination of 20 Sulfonylurea Herbicides in Soil by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

A method for the rapid determination of 20 sulfonylurea herbicides in soil by ultra-high performance liquid chromatography/tandem mass spectrometry was developed in this paper. The soil was freeze-dried, crushed and sifted, extracted with an accelerated solvent apparatus(ASE), purified by gel permeation chromatography (GPC), and then qualitatively and quantitatively analyzed by UPLC-MS/MS multi-stage monitoring mode (MRM) external standard method. The results showed that the detection limit of 20 sulfonylurea herbicides in soil was 2-5 ng/kg. Three standard recovery tests with different concentrations (1,5, 10 g/L) were carried out for the same environmental sample. The average recovery was 65.7%-106.1%, and the relative standard deviation was 2.3%-12.1%. This method is rapid, sensitive and accurate, and can be effectively applied to the rapid monitoring of 20 kinds of sulfonylurea herbicides in soil.