National Measurement Institute Australia has over 25 years’ experience producing certified reference materials (CRMs) to support national and international sports doping control laboratories. The 2000 Sydney Olympics prompted the on-going development of a comprehensive catalogue of calibration standards and isotopically labelled internal standards of interest to the WADA accredited laboratories, including metabolites of endogenous and exogenous steroids, stimulants, beta-blockers, selective androgen and estrogen receptor modulators, growth promotors and metabolites.
In-house synthesis has delivered human metabolites of varying structural complexity, confirmation of structure being established by synthesis precedent and key spectroscopic techniques, 1-D and 2-D NMR supported by mass spectrometry and infrared spectroscopy. Indicative purity value can be assigned by a standalone chromatographic technique (GC-FID or HPLC-UV-ELSD-CAD) to afford a reference material (RM) suitable for qualitative analysis. Certified reference materials (CRMs) with full mass balance and/or quantitative NMR assigned purity values stated as a mass fraction with established metrological traceability to the SI unit for mass (kg) are developed for accurate quantitative analysis.
Accreditation to ISO 17034 General requirements for the competence of reference material producers provides confidence that the reference material production is undertaken with an appropriate quality system in place. Participation in international comparison studies with other national metrology institutes demonstrates on-going capability in the purity assignment of compounds with molecular weights up to 900 g mol-1 with fit for purpose uncertainties down to ± 0.3% mass fraction.