Journal
ANALYTICA CHIMICA ACTA
Volume 756, Issue -, Pages 23-29Publisher
ELSEVIER
DOI: 10.1016/j.aca.2012.10.013
Keywords
Androgens; Isotope ratio mass spectrometry (IRMS); HPLC; Sample preparation; Doping in sports
Categories
Funding
- WADA [10A24XD]
Ask authors/readers for more resources
The confirmation by GC/C/IRMS of the exogenous origin of pseudo-endogenous steroids from human urine samples requires extracts of adequate purity. A strategy based on HPLC sample purification prior to the GC/C/IRMS analysis of human urinary endogenous androgens (i.e. testosterone, androsterone and/or androstenediols). is presented. A method without any additional derivatization step is proposed, allowing to simplify the urine pretreatment procedure, leading to extracts free of interferences permitting precise and accurate IRMS analysis, without the need of correcting the measured delta values for the contribution of the derivatizing agent. The HPLC extracts were adequately combined to both reduce the number of GC/C/IRMS runs and to have appropriate endogenous reference compounds (ERC; i.e. pregnanediol, 11-keto-etiocholanolone) on each GC-IRMS run. The purity of the extracts was assessed by their parallel analysis by gas chromatography coupled to mass spectrometry, with GC conditions identical to those of the GC/C/IRMS assay. The method has been validated according to ISO17025 requirements (within assay precision below 0.3 parts per thousand C-13 delta units and between assay precision below 0.6 parts per thousand C-13 delta units for most of the compounds investigated) fulfilling the World Anti-Doping Agency requirements. (C) 2012 Elsevier B.V. All rights reserved.
Authors
I am an author on this paper
Click your name to claim this paper and add it to your profile.
Reviews
Recommended
No Data Available