Accreditation and Quality Assurance

, Volume 12, Issue 9, pp 475–482

A high-accuracy method of analysis of 19-norandrosterone in human urine as utilised for the international laboratory intercomparison CCQM-P68

  • Lindsey G. Mackay
  • Daniel Burke
  • Fong-Ha Liu
  • Nigel Sousou
  • Veronica V. Vamathevan
  • Judy Cuthbertson
  • Chris Mussell
  • Richard B. Myors
Practitioner's Report

Abstract

A high-accuracy exact-matching isotope dilution mass spectrometry (IDMS) method for 19-norandrosterone (19-NA) in human urine was developed at NMIA for the certification of a freeze-dried human urine reference material (CRM NMIA MX002). The method utilised GC/HRMS analysis following hydrolysis, solvent extraction, HPLC fractionation and derivatisation. The method development included investigation of all potential analytical biases for the different stages of the method and included development of a confirmatory LC/MS/MS method. The measurement uncertainty of the reference method was rigorously investigated with the achieved expanded uncertainty being less than 4% at the 95% level of confidence. The method was used in the Comité Consultatif pour la Quantité de Matière (CCQM) pilot study CCQM-P68 which was an interlaboratory intercomparison for the analysis of 19-NA in human urine in which four national metrology institutes (NMIs) participated in. The agreement in the results from the NMIA method with those from the other NMIs was excellent.

Keywords

Steroids Nandrolone 19-Norandrosterone Urine Reference method Isotope dilution mass spectrometry Certified reference material 

References

  1. 1.
    WADA Technical Document—TD2004NA Reporting Norandrosterone Findings, WADA Laboratory Committee, 13 August 2004, http://www.wada-ama.org
  2. 2.
    Mackay LG, Burke D, Liu FH, Sousou N, Cuthbertson J, Vamathevan VV, Myors RB (2006) In: Schänzer W, Geyer H, Gotzmann A, Mareck U (eds) Recent advances in doping analysis, vol 14. Sportverlag Strauss, Köln, pp 203–211Google Scholar
  3. 3.
    Mackay LG, Burke D, Liu FH, Sousou N, Cuthbertson J (2006) In: Schänzer W, Geyer H, Gotzmann A, Mareck U (eds) Recent advances in doping analysis, vol 14. Sportverlag Strauss, Köln, pp 219–228Google Scholar
  4. 4.
    De Bièvre P, Peiser HS (1997) Fresenius J Anal Chem 359:523–525CrossRefGoogle Scholar
  5. 5.
    Mackay LG, Burke D, Welch MJ, Tai S, Mussell C, O’Connor G, Sin D, Wing WC (2007) Accred Qual Assur. doi:10.1007/s00769-007-0287-0Google Scholar
  6. 6.
    Mackay LG, Taylor CP, Myors RB, Hearn R, King B (2003) Accred Qual Assur 8:191–193Google Scholar
  7. 7.
    Henrion A (1994) Fresenius J Anal Chem 350:657–658CrossRefGoogle Scholar
  8. 8.
    Schanzer W, Donike M (1993) Anal Chim Acta 275:23–48CrossRefGoogle Scholar
  9. 9.
    ISO Guide to the Expression of Uncertainty in Measurement (1995) International Organization for Standardization, Geneva, SwitzerlandGoogle Scholar

Copyright information

© Springer-Verlag 2007

Authors and Affiliations

  • Lindsey G. Mackay
    • 1
  • Daniel Burke
    • 1
  • Fong-Ha Liu
    • 1
  • Nigel Sousou
    • 1
  • Veronica V. Vamathevan
    • 1
  • Judy Cuthbertson
    • 1
  • Chris Mussell
    • 2
  • Richard B. Myors
    • 1
  1. 1.National Measurement Institute, Australia (NMIA)PymbleAustralia
  2. 2.LGCMiddlesexUK

Personalised recommendations