Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Leioa, Basque Country, Spain; Research Centre for Experimental Marine Biology and Biotechnology (PIE), University of the Basque Country (UPV/EHU), Plentzia, Basque Country, Spain.
Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Leioa, Basque Country, Spain.
Sci Total Environ. 2022 Dec 1;850:157985. doi: 10.1016/j.scitotenv.2022.157985. Epub 2022 Aug 17.
An effect-directed analysis (EDA) approach was used to identify the compounds responsible for endocrine disruption in a hospital effluent (Basque Country). In order to facilitate the identification of the potentially toxic substances, a sample was collected using an automated onsite large volume solid phase extraction (LV-SPE) system. Then, it was fractionated with a two-step orthogonal chromatographic separation and tested for estrogenic effects with a recombinant yeast (A-YES) in-vitro bioassay. The fractionation method was optimized and validated for 184 compounds, and its application to the hospital effluent sample allowed reducing the number of unknowns from 292 in the raw sample to 35 after suspect analysis of the bioactive fractions. Among those, 7 of them were confirmed with chemical standards. In addition, target analysis of the raw sample confirmed the presence of mestranol, estrone and dodemorph in the fractions showing estrogenic activity. Predictive estrogenic activity modelling using quantitative structure-activity relationships indicated that the hormones mestranol (5840 ng/L) and estrone (128 ng/L), the plasticiser bisphenol A (9219 ng/L) and the preservative butylparaben (1224 ng/L) were the main contributors of the potential toxicity. Derived bioanalytical equivalents (BEQs) pointed mestranol and estrone as the main contributors (56 % and 43 %, respectively) of the 50 % of the sample's explained total estrogenic activity.
采用效应导向分析（EDA）方法来确定导致医院废水内分泌干扰的化合物（巴斯克地区）。为了方便鉴定潜在的有毒物质，使用自动化现场大体积固相萃取（LV-SPE）系统采集了一个样本。然后，采用两步正交色谱分离进行了馏分，并用重组酵母（A-YES）体外生物测定法测试了雌激素效应。该馏分方法经过优化和验证，可分析 184 种化合物，将其应用于医院废水样品，可将原始样品中的未知物数量从 292 种减少到生物活性馏分可疑分析后的 35 种。其中，有 7 种通过化学标准得到了确认。此外，原始样品的靶向分析证实了在显示雌激素活性的馏分中存在美雌醇、雌酮和 dodemorph。使用定量构效关系进行预测性雌激素活性建模表明，激素美雌醇（5840ng/L）和雌酮（128ng/L）、增塑剂双酚 A（9219ng/L）和防腐剂丁基对苯二酚（1224ng/L）是潜在毒性的主要贡献者。衍生的生物分析等效物（BEQs）表明，美雌醇和雌酮是样本总雌激素活性的 50%的主要贡献者（分别为 56%和 43%）。
