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Assessment of automated off-line solid-phase extraction LC-MS/MS to monitor EPA priority endocrine disruptors in tap water, surface water, and wastewater.

Authors
  • Goeury, Ken1
  • Vo Duy, Sung2
  • Munoz, Gabriel2
  • Prévost, Michèle3
  • Sauvé, Sébastien4
  • 1 Department of Chemistry, Université de Montréal, Montreal, QC, Canada; Department of Civil, Geological and Mining Engineering, École Polytechnique de Montréal, Montreal, QC, Canada. , (Canada)
  • 2 Department of Chemistry, Université de Montréal, Montreal, QC, Canada. , (Canada)
  • 3 Department of Civil, Geological and Mining Engineering, École Polytechnique de Montréal, Montreal, QC, Canada. , (Canada)
  • 4 Department of Chemistry, Université de Montréal, Montreal, QC, Canada. Electronic address: [email protected] , (Canada)
Type
Published Article
Journal
Talanta
Publication Date
May 01, 2022
Volume
241
Pages
123216–123216
Identifiers
DOI: 10.1016/j.talanta.2022.123216
PMID: 35042051
Source
Medline
Keywords
Language
English
License
Unknown

Abstract

EPA method 539.1 recently introduced an expanded list of priority endocrine-disrupting compounds (EDCs), some of which were also included in the Unregulated Contaminant Monitoring Rule 3 (UCMR3). Though standardized methods are available for drinking water, analysis of steroid hormones and bisphenol A (BPA) at the ultra-trace level remains challenging. This study set out to evaluate the suitability of automated off-line solid-phase extraction (SPE) liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) for the determination of EPA-priority EDCs in environmental water matrixes (tap water, surface water, and wastewater influents and effluents). The target molecules included 14 steroid hormones (altrenogest, androstenedione, equilenin, equilin, α-estradiol, β-estradiol, estriol, estrone, ethinylestradiol, levonorgestrel, medroxyprogesterone, norethindrone, progesterone, testosterone) and BPA. Factors that may influence the analytical performance were assessed. This involved, for instance, testing combinations of SPE materials from different brands and protocol variations. Several materials presented absolute extraction efficiencies in acceptable ranges. Initial sample pH, nature of reconstitution medium, and mobile phase salt concentration were among the potential factors affecting analyte signal. Storage conditions (different preservative agents) possibly exerted the strongest influence, in agreement with the literature. Limits of detection were in the range of 0.03-0.5 ng/L in drinking water, 0.1-0.5 ng/L in surface water, and 0.16-1 ng/L in wastewater. Method validation also involved testing linearity, accuracy, and precision in reagent water and matrix-matched extracted calibrants. The method was applied to field-collected water samples in Eastern Canada. Summed EDC concentrations remained low in tap water (<LOQ-0.92 ng/L), while higher detection frequencies and contamination levels were reported in riverine surface waters (2.6-37 ng/L) and municipal wastewaters (10-424 ng/L). Copyright © 2022 Elsevier B.V. All rights reserved.

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