超声波萃取-SPE净化-双柱双检测器测定土壤和沉积物中的20种有机氯

Determination of 20 organochlorine pesticides in soil and sediment by ultrasonic wave extraction-SPE cleanup-gas chromatography combined with dual-column and dual-ECD

建立了超声波萃取-SPE硅胶小柱净化-双柱双检测器气相色谱法测定土壤和沉积物中20种有机氯农药的方法。样品中添加高纯铜粉除硫,二氯甲烷超声萃取9 min,使用SPE硅胶小柱,9 mL丙酮:正己烷(1:9)洗脱净化。采用单进样口,双色谱柱双μ-ECD同时分离测定。土壤和沉积物样品中的方法检出限为0.001 mg/kg,平均回收率为73.17%～112.5%,相对标准偏差为0.33%～16%。

The determination method of 20 organochlorine pesticides in soil and sediment by ultrasonic wave extraetion-SPE silica column cleanup-gas chromatography combined with dual-column and dual-ECD was proposed. High-purified copper powder was added into the sample to remove sulfur. The sample was extracted by ultrasonic wave with CH2C12 for 9 minutes and purified by SPE silica column with 9 mL of acetone：hexane （ 1 ： 9）. Single injector, dual-column and dual-ECD were adopted to detect the target compounds. The detetion limit of method was 0. 001 mg/kg, deviations were from 0. 33% average recoveries were in the range of 73.17% -112. 5% and relative standard to 16%.