Development of anabolic–androgenic steroids purity certified reference materials for anti-doping

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BackgroundThe need for certified reference materials (CRM) of anabolic–androgenic steroids reference materials was emphasized by the Beijing 2008 Olympic game as a tool to improve comparability, ensuring accuracy and traceability of analytical results for competing athletes. The China National Institute of Metrology (NIM) responded to the state request by providing seven anabolic–androgenic steroids (AAS) reference materials for Beijing Olympic anti-doping, GBW (E) 100086–GBW (E) 100092.ExperimentalThis work describes the production of the series of AAS CRMs, according to ISO Guides 34 and 35 [1,2], which comprises the material processing, homogeneity and stability assessment, CRMs’ characterization including moisture content, trace metal content. The AASs’ purity values were assigned with collaborative study involved eight laboratories applying high resolution liquid chromatography-diode array detector (HPLC-DAD). Homogeneity of the AAS CRMs were determined by an in-house validated liquid chromatographic methodology. Potential degradation during storage was also investigated and a shelf-life based on this value was established.ResultsThe certified values of CRMs were 99.76 ± 0.079%, 99.76 ± 0.25%, 99.63 ± 0.09%, 99.67 ± 0.11%, 98.82 ± 0.56%, 96.30 ± 0.39% and 99.71 ± 0.49% (purity ± expanded uncertainty with confidence level of 95%) for methyltestosterone, testosterone propionate, nandrolone, nandrolone 17-propionate, boldenone, trenbolone acetate and testosterone respectively.ConclusionsThe certified values for all the studied AAS reference materials are traceable to the international system of units (SI). The CRMs developed were applied by 32 laboratory including sports organizations and analytical laboratories during the 2008 Olympic game for anti-doping control.Highlights▸ Seven anabolic–androgenic steroids certified references were developed. ▸ The purities were collaboratively assigned in eight laboratories via HPLC-DAD. ▸ All the studied AAS reference materials are traceable SI. ▸ The CRMs developed were applied by 32 field laboratory during the Beijing 2008.

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