凝胶色谱-固相萃取-气相色谱-串联质谱法测定水产品中9种三嗪类除草剂

建立了水产品中9种三嗪类除草剂的凝胶色谱 固相萃取-气相色谱-串联质谱(GPC-SPE-GC-MS/MS)分析方法。样品采用乙酸乙酯提取，凝胶渗透过滤，石墨化碳串联氨基柱净化，选择离子监测模式测定，外标法定量。结果表明：扑灭津、阿特拉津、特丁津、西玛津、扑草净在1.0~50.0 μg/L范围内线性良好，检出限均为1.0 μg/kg，在1.0~10.0 μg/kg添加水平，平均回收率为86.3%~119%，相对标准偏差为5.11%~10.1%；环草津、莠灭净、特丁净、西草净在2.0~100.0 μg/L范围内线性良好，检出限均为2.0 μg/kg，在2.0~20.0 μg/kg添加水平，平均回收率为87.6%~112%，相对标准偏差为5.27%~9.56%。该方法稳定、可靠，适用于水产品中9种三嗪类除草剂的同时测定。

Determination of 9 Triazine Herbicides in Aquatic Products by GPC-SPE-GC-MS/MS

A method for determination of 9 triazine herbicides residues in aquatic products by gel permeation chromatography-solid phase extraction-gas chromatography tandem mass spectrometry(GPC-SPE-GC-MS/MS) was established. The sample was extracted with ethyl acetate, then cleaned up by gel permeation chromatography and purified by carbon and NH₂ solid phase extraction column. The analytes were determined in selected ion monitoring and quantified by external method. Propazine, atrazine, terbuthylazine, simazine and cyprazine show good linearity in the range of 1.0-50.0 μg/L, and the detection limits of the five analytes are 1.0 μg/kg. The average recoveries range from 86.3% to 119% when spiked at 1.0-10.0 μg/kg with relative standard deviations from 5.11% to 10.1%. Simetryn, prometryn, ametryn and terbutryn show good linearity in the range of 2.0-100.0 μg/L, and the detection limits are 2.0 μg/kg. The average recoveries range from 87.6% to 112% when spiked at 2.0-20.0 μg/kg with relative standard deviations from 5.27% to 9.56%. The method is stable and reasonable, and which can be used for the determination of 9 triazine herbicides residues in aquatic products.