Zarzycki Paweł K, Włodarczyk Elzbieta, Baran Michał J
Section of Toxicology and Bioanalytics, Department of Environmental Biology, Koszalin University of Technology, Sniadeckich 2, 75-453 Koszalin, Poland.
J Chromatogr A. 2009 Oct 30;1216(44):7612-22. doi: 10.1016/j.chroma.2009.03.066. Epub 2009 Mar 28.
In the present work solid-phase extraction protocol based on C18 tubes and organic water washing solvents as well as isocratic HPLC procedure focused on quantification of free steroids and related low-molecular-mass endocrine disrupting compounds (EDCs), characterized by different polarity varied from estetrol to progesterone, were studied. Described separation method involves temperature-dependent inclusion chromatography with mobile phase modified with beta-cyclodextrin. Using such analytical approach the environmental samples derived from Baltic Sea, selected lakes and rivers of the Middle Pomerania in northern part of Poland as well as untreated and treated sewage water from municipal sewage treatment plant near Koszalin were analyzed. Moreover, some preliminary data concerning estriol, testosterone and equilin biodegradation involving activated sludge material were reported. Cluster and principal components analysis of the acquired data sets confirms a high separation and quantification throughput of the solid-phase extraction and isocratic HPLC protocols presented. The method can be useful for simple and rapid classification of the environmental samples characterized by different sources of EDCs loading. The results of this work extend the utility of temperature-dependent inclusion chromatography as an inexpensive, efficient and accurate analytical tool appropriate for characterisation and quantification of complex environmental samples.
在本研究中，对基于C18管和有机水洗溶剂的固相萃取方案以及等度高效液相色谱法进行了研究，该方法着重于对游离类固醇和相关低分子量内分泌干扰化合物（EDC）进行定量分析，这些化合物具有从雌三醇到孕酮不等的不同极性。所描述的分离方法涉及温度依赖性包合色谱法，其流动相用β-环糊精进行了改性。采用这种分析方法，对源自波罗的海、波兰北部中波美拉尼亚选定的湖泊和河流的环境样品以及科沙林附近城市污水处理厂未经处理和经处理的污水进行了分析。此外，还报告了一些关于涉及活性污泥材料的雌三醇、睾酮和马萘雌酮生物降解的初步数据。对所获取数据集的聚类分析和主成分分析证实了所提出的固相萃取和等度高效液相色谱方案具有高分离和定量通量。该方法可用于对具有不同EDC负荷来源的环境样品进行简单快速的分类。本研究结果扩展了温度依赖性包合色谱法作为一种廉价、高效且准确的分析工具的用途，该工具适用于对复杂环境样品进行表征和定量分析。
