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Certification of methylmercury content in two fresh-frozen reference materials: SRM 1947 Lake Michigan fish tissue and SRM 1974b organics in mussel tissue (Mytilus edulis)

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Abstract

This paper describes the development of two independent analytical methods for the extraction and quantification of methylmercury from marine biota. The procedures involve microwave extraction, followed by derivatization and either headspace solid-phase microextraction (SPME) with a polydimethylsiloxane (PDMS)-coated silica fiber or back-extraction into iso-octane. The identification and quantification of the extracted compounds is carried out by capillary gas chromatography/mass spectrometric (GC/MS) and inductively coupled plasma mass spectrometric (GC/ICP-MS) detection. Both methods were validated for the determination of methylmercury (MeHg) concentrations in a variety of biological standard reference materials (SRMs) including fresh-frozen tissue homogenates of SRM 1946 Lake Superior fish tissue and SRM 1974a organics in mussel tissue (Mytilus edulis) and then applied to the certification effort of SRM 1947 Lake Michigan fish tissue and SRM 1974b organics in mussel tissue (Mytilus edulis). While past certifications of methylmercury in tissue SRMs have been based on two independent methods from the National Institute of Standards and Technology (NIST) and participating laboratories, the methods described within provide improved protocols and will allow future certification efforts to be based on at least two independent analytical methods within NIST.

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Acknowledgements

WCD acknowledges financial support from the National Institute of Standards and Technology National Research Council Postdoctoral Research Associateship Program. Certain commercial equipment, instruments, and materials are identified in this paper to adequately specify the experimental procedure. Such identification does not imply recommendation or endorsement by NIST nor does it imply that the equipment, instruments, or materials are necessarily the best available for the purpose.

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Authors and Affiliations

  1. Hollings Marine Laboratory, Analytical Chemistry Division, National Institute of Standards and Technology (NIST), 331 Fort Johnson Road, Charleston, SC, 29412, USA

    W. Clay Davis, S. J. Christopher, Rebecca S. Pugh & David Point

  2. LCABIE/CNRS Hélioparc Pau-Pyrénées, 2 Avenue P. Angot, 64053, Pau Cedex 9, France

    O. F. X. Donard, Eva A. Krupp & David Point

  3. Jožef Stefan Institute, Jamova, 39, 1000, Ljubljana, Slovenia

    Milena Horvat, D. Gibičar & Z. Kljakovic-Gaspic

  4. Institute for Medical Research and Occupational Health, Ksaverska cesta 2, 10000, Zagreb, Croatia

    Z. Kljakovic-Gaspic

  5. Analytical Chemistry Division, National Institute of Standards and Technology (NIST), Gaithersburg, MD, 20899, USA

    Barbara J. Porter & Michele M. Schantz

Authors
  1. W. Clay Davis
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  2. S. J. Christopher
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  3. Rebecca S. Pugh
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  4. O. F. X. Donard
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  5. Eva A. Krupp
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  6. David Point
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  7. Milena Horvat
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  8. D. Gibičar
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  9. Z. Kljakovic-Gaspic
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  10. Barbara J. Porter
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  11. Michele M. Schantz
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Correspondence to W. Clay Davis.

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Davis, W.C., Christopher, S.J., Pugh, R.S. et al. Certification of methylmercury content in two fresh-frozen reference materials: SRM 1947 Lake Michigan fish tissue and SRM 1974b organics in mussel tissue (Mytilus edulis). Anal Bioanal Chem 387, 2335–2341 (2007). https://doi.org/10.1007/s00216-006-1106-x

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  • DOI: https://doi.org/10.1007/s00216-006-1106-x

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