加速溶剂萃取-气相色谱法测定土壤中有机氯农药和多氯联苯
Determination of Organochlorine Pesticides and Polychlorinated Biphenyls in Soils by Gas Chromatography with Accelerated Solvent Extraction
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摘要: 试验了加速溶剂萃取土壤中有机氯农药和多氯联苯残留的最佳条件。结果表明,采用正己烷-丙酮混合溶剂(体积比1∶1)为提取剂,萃取温度100℃,压力为10.3 MPa; 采用弗罗里硅土固相萃取柱对样品净化,毛细管柱分离,用配有电子捕获检测器的气相色谱进行检测,平均加标回收率为83.6%~109.0%,相对标准偏差(RSD,n=11)为1.11%~5.88%,检出限为0.69~1.85 ng/g。方法简单、快捷、经济,适应于土壤中的有机氯农药和多氯联苯的测定。Abstract: The optimum extraction condition was studied for organochlorine pesticides and polychlorinated biphenyls in soils using accelerated solvent extraction (ASE). The sample was extracted with hexane/acetone (1∶ 1, V/V) with extraction temperature of 100℃ and pressure of 10.3 MPa and cleaned up by solid phase extraction with Florisil column, followed by separation on a capillary column. The target organic pollutants were then quantitatively determined by gas chromatography using electron capture detection. The detection limits of the method was 0.69~1.85 ng/g and average recovery was 83.6%~109.0% with precision of 1.11%~5.88% RSD (n=11). The method is simple, efficient, economical and suitable for the analysis of organochlorine pesticides and polychlorinated biphenyls in soil samples.