Abstract
This manuscript presents a comprehensive analytical framework for identification and quantification of chemically diverse endocrine disrupting chemicals (EDCs) used in personal care and consumer products in diverse solid and liquid environmental matrices with an ultimate goal of evaluating public exposure to EDCs via water fingerprinting. Liquid chromatography coupled with tandem quadrupole time-of-flight mass spectrometry (UHPLC-ESI-MS/MS) was used for targeted analysis of selected EDCs as well as to identify and quantify a few metabolites using post-acquisition data mining. Solid-phase extraction (SPE) was applied to liquid matrices in order to reduce matrix effects and provide required sample concentration and ultimately, high sensitivity and selectivity of measurements. SPE recoveries in liquid samples ranged from 49 to 140% with method quantification limits not exceeding 1 ng L−1 for the majority of EDCs. Microwave-assisted extraction (MAE) was applied to solid samples and when followed by SPE, it permitted the analysis of EDCs in digested sludge. MAE/SPE recoveries varied from 11 to 186% and MQLs between 0.03 and 8.1 ng g−1 with the majority of compounds showing MQLs below 2 ng g−1. Mass error for quantifier and qualifier ions was below 5 ppm when analysing river water and effluent wastewater and below 10 ppm when analysing influent wastewater and solid samples. The method was successfully applied to environmental samples, with 33 EDCs identified and quantified in wastewater and receiving waters. In addition, several EDCs were found in digested sludge, which confirms that for a more comprehensive understanding of exposure patterns and environmental impact, analysis of solids cannot be neglected. Finally, post-acquisition data mining permitted the identification and quantification of a metabolite of BPA and the identification of a metabolite of 4-Cl-3-methylphenol.Graphical abstractᅟ
Highlights
IntroductionSeveral studies have investigated the presence of endocrine disrupting chemicals (EDCs) in different types of samples including surface waters, wastewater, digested sludge and solid samples [10,11,12,13,14,15,16,17,18,19]
Many chemicals in personal care and consumer products such as preservatives, UV filters, plasticizers, fragrances, antimicrobials, pesticides and flame retardants are suspected to haveElectronic supplementary material The online version of this article contains supplementary material, which is available to authorized users.or are recognised as endocrine system disruptors [1, 2]
The following analytes were targeted in this study (see Electronic Supplementary Material (ESM) Table S1): 2,4,5trichlorophenol, 2,4,6-trichlorophenol, 2-ethylhexanoic acid, 2-naphthol, 4,4′-dihydroxybenzophenone, 4-benzylphenol, 4-chloro-3,5,dimethylphenol, 4-chloro-3-methylphenol, 4-nnonylphenol, 4-n-octylphenol, atrazine, benzophenone-1 (BP-1), benzophenone-2 (BP-2), benzophenone-3 (BP-3), benzophenone-4 (BP-4), benzylparaben, bisphenol A (BPA), bisphenol A bis(3-chloro-2-hydroxypropyl) ether (BADGE2-Cl), butylparaben, chlorothymol, dibutyl phthalate (DBP), ethylparaben, galaxolide, 1,2,5,6,9,10-hexabromocyclododecane (HBCD), mono(2-ethylhexyl)phthalate (MEHP), methylparaben, monobutyl phthalate (MBP), musk ketone, padimate O, perfluorooctanesulfonic acid (PFOS), perfluorooctanoic acid (PFOA), phenylbenzimidazolesulfonic
Summary
Several studies have investigated the presence of EDCs in different types of samples including surface waters, wastewater, digested sludge and solid samples [10,11,12,13,14,15,16,17,18,19] These studies have utilised different analytical techniques for both sample preparation, separation and detection. Most of these studies focussed on a small number of EDCs generally from a limited number of chemical classes [21,22,23,24] and/or are often investigated alongside other pharmaceuticals [14, 17, 19, 25,26,27] These studies used targeted MS detection meaning that their results cannot be used for retrospective data analysis
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