Analytical and Bioanalytical Chemistry

, Volume 387, Issue 7, pp 2335–2341 | Cite as

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)

  • W. Clay DavisEmail author
  • S. J. Christopher
  • Rebecca S. Pugh
  • O. F. X. Donard
  • Eva A. Krupp
  • David Point
  • Milena Horvat
  • D. Gibičar
  • Z. Kljakovic-Gaspic
  • Barbara J. Porter
  • Michele M. Schantz
Original Paper


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.


Speciation Organometals Certified reference material 



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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Copyright information

© Springer-Verlag 2007

Authors and Affiliations

  • W. Clay Davis
    • 1
    Email author
  • S. J. Christopher
    • 1
  • Rebecca S. Pugh
    • 1
  • O. F. X. Donard
    • 2
  • Eva A. Krupp
    • 2
  • David Point
    • 1
    • 2
  • Milena Horvat
    • 3
  • D. Gibičar
    • 3
  • Z. Kljakovic-Gaspic
    • 3
    • 4
  • Barbara J. Porter
    • 5
  • Michele M. Schantz
    • 5
  1. 1.Hollings Marine Laboratory, Analytical Chemistry DivisionNational Institute of Standards and Technology (NIST)CharlestonUSA
  2. 2.LCABIE/CNRS Hélioparc Pau-PyrénéesPau Cedex 9France
  3. 3.Jožef Stefan InstituteLjubljanaSlovenia
  4. 4.Institute for Medical Research and Occupational HealthZagrebCroatia
  5. 5.Analytical Chemistry DivisionNational Institute of Standards and Technology (NIST)GaithersburgUSA

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