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

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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.

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Acknowledgments

The authors are highly grateful to the World Anti-Doping Agency (WADA) and the Australian Government’s Anti-Doping Research Program for their financial support for this work. The authors would also like to thank the German Sport University, Cologne, for providing, via WAADS, a solution of the D4-19-NAG internal standard.

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Authors and Affiliations

  1. National Measurement Institute, Australia (NMIA), 1 Suakin Street, Pymble, NSW, 2073, Australia

    Lindsey G. Mackay, Daniel Burke, Fong-Ha Liu, Nigel Sousou, Veronica V. Vamathevan, Judy Cuthbertson & Richard B. Myors

  2. LGC, Queens Road, Teddington, Middlesex, TW11 0LY, UK

    Chris Mussell

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  1. Lindsey G. Mackay
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  2. Daniel Burke
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  3. Fong-Ha Liu
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  4. Nigel Sousou
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  5. Veronica V. Vamathevan
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  6. Judy Cuthbertson
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  7. Chris Mussell
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  8. Richard B. Myors
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Correspondence to Lindsey G. Mackay.

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Mackay, L.G., Burke, D., Liu, FH. et al. A high-accuracy method of analysis of 19-norandrosterone in human urine as utilised for the international laboratory intercomparison CCQM-P68. Accred Qual Assur 12, 475–482 (2007). https://doi.org/10.1007/s00769-007-0288-z

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  • DOI: https://doi.org/10.1007/s00769-007-0288-z

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