土壤中持久性有机污染物分析的前处理方法
Pre-treatment Methods for Analysis of Persistent Organic Pollutants in Soil Samples
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摘要: 对土壤样品的前处理技术进行了研究.采用加速溶剂萃取法(ASE)提取土壤中有机氯农药和多氯联苯类化合物,并且与索氏提取结果进行了对比,结果表明,ASE完全能取代传统的索氏提取方法.对固相萃取(SPE)柱净化的不同填料进行了实验筛选.比较了浓硫酸磺化法和SPE柱净化法对土壤中有机氯农药及多氯联苯的净化效果.优化了有机氯农药、多氯联苯凝胶渗透色谱(GPC)的净化条件.当样品基质比较复杂时,采用凝胶渗透色谱结合固相萃取柱的前处理方法,能得到很好的净化效果.土壤样品中持久性有机污染物采用加速溶剂提取结合固相萃取前处理过程的回收率为68%～106%,精密度小于7.7%.Abstract: In this paper, the study on pre-treatment technology for analysis of persistent organic pollutants in soil samples was reported. Accelerated solvent extraction(ASE) method was used to extract organochlorine pesticides and polychlorinated biphenyls in soil samples and the results were compared with those from Soxhlet extraction（SE） method. It indicates that ASE can substitute for traditional SE method in extraction of persistent organic pollutants in soil samples. Different sorbents for cleanup column used in solid phase extraction(SPE) were selected by the experiments and the cleanup effect for organochlorine pesticides and polychlorinated biphenyls in soil samples by SPE and sulphonation method were compared. The clean-up condition for gel permeation chromatography(GPC) was also optimized. The results of the study show that the method of GPC combined with SPE is suitable for the pretreatment of soil samples with complicated matrix. And the average recoveries for the method of ASE combined with SPE is 68%~106% with the precision of less than 7.7%RSD.
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