气相色谱法测定土壤中德克隆

Determination of Dechlorane Plus in Soil by Gas Chromatography

采用索氏提取-气相色谱电子捕获检测器分析土壤中顺式-德克隆和反式-德克隆含量。对索氏提取和柱净化条件进行优化,得到最优条件为:采用二氯甲烷-正己烷混合溶剂(体积比为1:1)进行索氏提取10 h后选用硅胶析柱净化,再用8 mL二氯甲烷洗脱。最优条件下进行土壤样品高、中、低浓度的加标实验,顺式-德克隆的加标回收率为90.2%~97.1%,反式-德克隆加标回收率为90.1%~91.4%,准确度和精密度较高。顺式-德克隆的方法检出限为0.14μg/kg,反式-德克隆方法检出限为0.09μg/kg。

Soxhlet extraction and gas chromatography electron capture detector were used to analyze the content of syn-and anti-Dechlorane Plus in soil.The conditions of Soxhlet extraction and column purification were optimized.The optimum conditions were obtained as follows:the mixed solvent of dichloromethane and nhexane(volume ratio was 1:1)was used for Soxhlet extraction for 10 hours,and silica gel column was used for purification,and then 8 mL of dichloromethane was used for elution.Under the optimal conditions,the spiking experiments of soil samples with high,medium and low concentrations were carried out.The spiking recoveries of syn-and anti-Dechlorane Plus were 90.2%~97.1%and 90.1%~91.4%,respectively,with high accuracy and precision.The detection limit of syn-Dechlorane Plus was 0.14μg/kg,and the detection limit of anti-Dechlorane Plus was 0.09μg/kg.