沉积物样品中干扰物的去除及多种持久性有机污染物气相色谱分析
A Gas Chromatography Method for Determination of Persistent Organic Pollutants in Sediment and the Research on the Removal of Contaminants
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摘要: 建立了沉积物样品中17种有机氯农药和8种多氯联苯持久性有机污染物的气相色谱分析方法。针对沉积物样品基质复杂、含有大量硫干扰的特点,重点研究了前处理技术。采用加速溶剂提取(ASE)技术提取样品中的有机污染物,比较了加入铜粉后ASE在线除硫和超声波提取除硫的效果。结果表明,加入铜粉ASE提取不能完全去除硫的干扰,需进一步采用超声波提取10 min除硫才能大大减少杂质对目标化合物的干扰。沉积物样品中的色素类及小分子干扰物质采用凝胶渗透色谱结合固相萃取技术进行净化,满足了气相色谱-电子捕获检测器分析的要求。25种化合物的平均添加回收率为68％~131％,方法精密度(RSD,n=6)小于22.3％,检出限为0.10~0.51 μg/kg。建立的样品前处理技术净化彻底,适合用于不同地区、不同类型的沉积物样品气相色谱分析。Abstract: Sediment matrices containing a large amount of sulfocompound are complex. In this paper, the pre-treatment methods for analysis of organic pollutants in sediment are presented. The extraction technology uses the accelerated solvent extraction (ASE) technique and different methods were compared to eliminate sulfocompound. The results indicate that the additional 10 minute step by ultrasonic extraction with copper powder is necessary. Gel permeation chromatography (GPC) combined with solid phase extraction (SPE) was used to clean-up. This pre-treatment method meets the requirements of analysis by Gas Chromatography-Electron Capture Detector (GC-ECD). The method for the determination of persistent organic pollutants including 17 organochlorine pesticides and 8 polychlorinated biphenyls in sediment by gas chromatography was established. The average recoveries of the 25 compounds ranged from 68% to 131%. The relative standard deviation (RSD) for all the compounds was lower than 22.3%. The minimum detection limits (MDL) were between 0.1 and 0.51 μg/kg. This method can remove most of the contaminants in co-extractions, minimize the possibility of releasing false positive results and can be applied in analysis of different types of sediment.
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Key words:
- sediment /
- organochlorine /
- pesticides /
- polychlorinated
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