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Drug testing data from the 2007 Pan American Games: δ 13C values of urinary androsterone, etiocholanolone and androstanediols determined by GC/C/IRMS

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PERGAMON-ELSEVIER SCIENCE LTD
DOI: 10.1016/j.jsbmb.2009.03.012

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Gas chromatography; Combustion; Isotope ratio mass spectrometry; Doping; Confirmation; Steroids; Pan American Games; C-13/C-12

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The main purpose of this article is to show the application of the CG/C/IRMS in real time during competition in the steroid confirmation analysis. For this reason, this paper summarizes the results obtained from the doping control analysis during the period of the 2007 Pan American Games held in Rio de Janeiro, Brazil. Approximately 5600 athletes from 42 different countries competed in the games. Testing was performed in accordance to World Anti-Doping Agency (WADA) technical note for prohibited substances. This paper reports data where abnormal urinary steroid profiles, have been found with the screening procedures. One 8 mL urine sample was used for the analysis of five steroid metabolites with two separate analyses by gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS). Urine samples were submitted to GC/C/IRMS for confirmation analysis to determine the C-13/C-12 ratio of selected steroids. Fifty-seven urine samples were analyzed by GC/C/IRMS and the delta C-13 values (parts per thousand) of androsterone, etiocholanclone, 5 beta-androstane-3 alpha, 17 beta-diol (5 beta-diol), 5 alpha-androstane-3 alpha, 1 beta p-diol (5 alpha-diol) and 5 beta-pregnane-3 alpha, 20 alpha-diol (5 beta-pdiol), the endogenous reference compound are presented. One urine sample with a testosterone/epitestosterone (T/E) ratio of 4.7 was confirmed to be positive of doping by GC/C/IRMS analysis. The delta values of 5 beta-diol and 5 alpha-diol were 3.8 and 10.8, respectively, compared to the endogenous reference compound 5 beta-pdiol, which exceeded the WADA limit of 3 parts per thousand. The results obtained by CG/C/IRMS confirmation analyses, in suspicious samples, were conclusive in deciding whether or not a doping steroid violation had occurred. (C) 2009 Elsevier Ltd. All rights reserved.

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