引用本文:陈永山,骆永明,章海波,宋 静,黄玉娟.土壤样品中酞酸酯含量分析的前处理研究——提取液浓缩过程与净化的影响[J].土壤学报,2011,48(2):311-319. DOI:10.11766/trxb200909060398
chenyongshan,luoyongming, , , .Pretreatment of soil samples for analysis of phthalate esters thereine[J].Acta Pedologica Sinica,2011,48(2):311-319. DOI:10.11766/trxb200909060398
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土壤样品中酞酸酯含量分析的前处理研究——提取液浓缩过程与净化的影响
陈永山, 骆永明, 章海波, 宋 静, 黄玉娟
中科院南京土壤研究所
摘要:
我国农田土壤酞酸酯污染时有报道,由于具有内分泌干扰作用而广受关注。本研究通过比较索氏提取和超声这两种提取土壤酞酸酯的方法,认为从提高回收率和降低背景干扰角度出发,超声提取法更合适作为土壤酞酸酯分析的前处理。针对超声提取过程中的一些操作步骤的细节做了比较研究,表明提取液不蒸干可减少酞酸酯的挥发损失,提取液过净化柱与否对GC-MS分析多数酞酸酯组分影响不大,不过净化柱处理可提高土壤酞酸酯的分析效率,但土壤中过多的色素干扰可能会影响某些组分(如邻苯二甲酸二(2-乙基)己酯)的分析结果。
关键词:  酞酸酯,索氏提取,超声提取,土壤
基金项目: 国家水体污染控制与治理科技重大专项课题 (2008ZX07101-006-05);中国科学院“优秀博士学位论文、院长奖获得者科研启动专项资金”
Pretreatment of soil samples for analysis of phthalate esters thereine
chenyongshan, luoyongming
Institute of Soil Science, Chinese Academy of Sciences
Abstract:
Contamination of phthalate esters (PAEs) in agricultural soils is reported frequently in China recently and has raised wide concern to researches due to the effects of endocrine disrupt. Ultrasonic extraction and Soxhlet extraction were both performed to extract the added PAEs from soil. The results indicated that the ultrasonic extraction was more feasible to be the pretreatment method for PAEs analysis of soil sample as a result of increasing recovery and decreasing procedure blank. Meanwhile, operating procedures of ultrasonic extraction were studied further, Preservation of 1-2ml of the extract instead of dryness will effectively prevent the loss of compounds from volatilization in the process of rotating evaporator. No obvious difference was observed between the treatment of cleanup and without cleanup by florisil when analyzed by GC-MS in present study. Skip of the cleanup process will increase the efficiency of PAEs analysis, however, the interference of pigment or other components in the soil samples will have an impact on the accuracy of Bis(2-ethylhexyl) phthalate (DEHP) and other target compouds.
Key words:  phthalate esters, ultrasonic extraction, soxhlet extraction, soil