采用气相色谱-微电子捕获检测器法,建立了吡氟酰草胺的仪器分析方法及其在土壤、水和沉积物等环境样品中的残留检测方法.使用HP-5MS柱建立微电子捕获检测气相色谱分析方法,样品经丙酮提取,乙酸乙酯萃取净化,外标法定量分析.结果表明:在0.05~1.0 mg·kg-1添加水平范围内,吡氟酰草胺的平均添加回收率为88.6%~105.9%,相对标准偏差(RSD)为1.5%~6.1%(n=5).方法的最小检出量(MDL)为1×10-10g,吡氟酰草胺在土壤、沉积物和水基质中的定量限(LOQ)均为0.005 mg·kg-1.该方法杂质干扰少,准确性及灵敏度满足农药残留检测要求,对检测硬件要求低,适用于土壤、沉积物和水等环境样品中吡氟酰草胺残留的分析.%A method for determination of dilflufenican residue in soil,water,and sediment samples was established based on gas chromatograph with microcell electron capture detector(GC-μECD). Residues were extracted from samples with acetone,followed extraction by ethyl acetate,and quantified by external standard method,determination using GC-μECD and HP-5MS column. Aver-age fortified recoveries in samples were found at the range of 88. 6%-105. 9%at fortified levels from 0. 05mg·kg-1 to 1. 0 mg· kg-1,with relative standard deviations of 1. 5%-6. 1%(n=5). The method detection limit(MDL)of dilflufenican was 1×10-10g,and the limit of quantification(LOQ)of dilflufenican in samples was 0. 005 mg·kg-1. No interferences were found by using this method for blank samples. The current method need no special instrument and can meet the requirements of pesticide residue analysis on accuracy,sensitivity and precision. In conclusion,this method is suitable for the analysis of dilflufenican residue in environmental samples such as soil,water,and sediment.
展开▼
