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    A sensitive liquid chromatography/tandem mass spectrometry method for the determination of natural and synthetic steroid estrogens in seawater and marine biota, with a focus on proposed Water Framework Directive Environmental Quality Standards

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    Ronan and McHugh. A sensitive ...
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    Author
    Ronan, J.
    McHugh, B.
    Keyword
    Spectrometry
    Estrogens
    Water Framework Directive
    Environmental Quality Standards
    WFD
    WFD, 2000/60/ EC
    Date
    2013
    Publisher
    Wiley
    
    Metadata
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    Abstract
    RATIONALE: Trace levels of natural and synthetic steroid estrogens estrone (E1), 17b-estradiol (E2) and 17a-ethynyl estradiol (EE2) have been demonstrated to exert adverse effects in exposed organisms. E2 and EE2 have been proposed for inclusion in the Water Framework Directive (WFD) list of priority pollutants; however, the detection and accurate quantification of these compounds provide significant challenges, due to the low detection limits required. METHODS: A sensitive method combining ultrasonication, solid-phase extraction (SPE) and liquid chromatography/tandem mass spectrometry, with electrospray ionisation in negative mode (LC/ESI-MS/MS), capable of determining E1, E2 and EE2 at concentrations between 0.07 and 60 ng/L for seawater and between 0.4 and 200 ng/g wet weight in Mytilus spp. is reported. Recoveries at the limit of quantification (LOQ) ranged from 95 to 102% and 88 to 100% for water and tissue, respectively. Salinity (12 to 35%) and typical marine particulate matter loadings (between 10 and 100 mg/L) were not found to affect analyte recoveries. RESULTS: The first detection of E1 by LC/MS/MS in Irish marine waters (Dublin Bay, at 0.76 ng/L) is reported. Steroids were not detected in Galway Bay, or in any mussel samples from Dublin, Galway and Clare. The level of E2 detected in the dissolved water phase was below the proposed WFD Environmental Quality Standard (EQS) in other surface waters. CONCLUSIONS: The proposed method is suitable for the detection of E1, E2 and EE2 at biologically relevant concentrations and, due to the specificity offered, is not subject to potential interferences from endogenous E1 and E2 which often complicate the interpretation of estrogenic biomarker assays.
    URI
    http://hdl.handle.net/10793/1281
    Description
    Peer-reviewed. This article may be used for non-commercial purposes in accordance with Wiley Terms and Conditions for Self-Archiving.
    Citation
    Ronan, J. and McHugh, B. (2013). A sensitive liquid chromatography/tandem mass spectrometry method for the determination of natural and synthetic steroid estrogens in seawater and marine biota, with a focus on proposed Water Framework Directive Environmental Quality Standards. Rapid communications in mass spectrometry, 27(7), pp. 738–746 doi:10.1002/rcm.6505
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