Abstract
The list of endocrine disrupting compounds (EDCs) defined under U.S. EPA Method 539 was recently expanded to include additional hormones and bisphenol A (BPA). Here, we validated a fast and robust alternative method compliant with Method 539.1 requirements in diverse water matrixes (i.e., ultra-pure water, tap water, surface water, and wastewater influent and effluent). Automated large volume injection solid phase extraction (SPE) coupled on-line to ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) was investigated for this purpose. The surveyed molecules included 13 EPA-priority hormones (testosterone, progesterone, medroxyprogesterone, levonorgestrel, norethindrone, androstenedione, estrone, β-estradiol, α-estradiol, equilin, equilenin, ethinylestradiol, estriol) and BPA. Combinations of ionization source and mobile phases were optimized for improved sensitivity. Suitable chromatographic performances were obtained and the implementation of an on-line SPE washing step consecutive to sample loading was investigated. On-line SPE extraction efficiencies in acceptable ranges (64–79%) and detection limits in the order of nanogram per liter or sub-nanogram per liter were obtained. The linearity range extended over 2–3 orders of magnitude, with determination coefficients (R2) typically > 0.9980. Robust precision and trueness complying with acceptance criteria (70–130%) were obtained for the scope of analytes/matrix combinations. Limited internal standard variations were also observed across samples (±18%), well within the ±50% acceptance criterion. The method was successfully applied to field-collected samples in Canada and summed EDC concentrations were reported in the range of 0.80–2.8 ng L−1, 6.8–19 ng L−1, 260–790 ng L−1, and 37–360 ng L−1 in tap water, surface water, effluent and influent wastewater samples, respectively.
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