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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Authors: | Lindsey G Mackay Daniel Burke Fong-Ha Liu Nigel Sousou Veronica V Vamathevan Judy Cuthbertson Chris Mussell Richard B Myors |
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Institution: | (1) National Measurement Institute, Australia (NMIA), 1 Suakin Street, Pymble, NSW, 2073, Australia;(2) LGC, Queens Road, Teddington, Middlesex, TW11 0LY, UK |
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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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Keywords: | Steroids Nandrolone 19-Norandrosterone Urine Reference method Isotope dilution mass spectrometry Certified reference material |
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