Validation and performance comparison of two carbon isotope ratio methods to control the misuse of androgens in humans
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- 作者：Christophe Saudan ; Caroline Emery ; Franç ; ois Marclay ; Emmanuel Strahm ; Patrice Mangin ; Martial Saugy
- 关键词：Method validation ; Isotope ratio mass spectrometry (IRMS) ; Testosterone misuse ; Doping control
- 刊名：Journal of Chromatography B, Analytical Technologies in the Biomedical and Life Sciences
- 出版年：2009
- 出版时间：1 August 2009
- 年：2009
- 卷：877
- 期：23
- 页码：2321-2329
- 全文大小：669 K
文摘
Carbon isotope ratio of androgens in urine specimens is routinely determined to exclude an abuse of testosterone or testosterone prohormones by athletes. Increasing application of gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS) in the last years for target and systematic investigations on samples has resulted in the demand for rapid sample throughput as well as high selectivity in the extraction process particularly in the case of conspicuous samples. For that purpose, we present herein the complimentary use of an SPE-based assay and an HPLC fractionation method as a two-stage strategy for the isolation of testosterone metabolites and endogenous reference compounds prior to GC/C/IRMS analyses. Assays validation demonstrated acceptable performance in terms of intermediate precision (range: 0.1–0.4‰) and Bland–Altman analyses revealed no significant bias (0.2 ‰). For further validation of this two-stage analyses strategy, all the specimens (n = 124) collected during a major sport event were processed.