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2.
J Steroid Biochem Mol Biol ; 115(3-5): 107-14, 2009 Jul.
Article in English | MEDLINE | ID: mdl-19428237

ABSTRACT

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 (13)C/(12)C ratio of selected steroids. Fifty-seven urine samples were analyzed by GC/C/IRMS and the delta(13)C values ( per thousand) of androsterone, etiocholanolone, 5beta-androstane-3alpha, 17beta-diol (5beta-diol), 5alpha-androstane-3alpha, 17beta-diol (5alpha-diol) and 5beta-pregnane-3alpha, 20alpha-diol (5beta-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 5beta-diol and 5alpha-diol were 3.8 and 10.8, respectively, compared to the endogenous reference compound 5beta-pdiol, which exceeded the WADA limit of 3 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.


Subject(s)
Anabolic Agents/urine , Androstanols/urine , Androsterone/urine , Doping in Sports , Etiocholanolone/urine , Mass Spectrometry/methods , Substance Abuse Detection/methods , Brazil , Carbon Isotopes/urine , Chromatography, Gas , Estrogens/urine , Female , Humans , Male , Quality Control , Specimen Handling , Testosterone/chemistry , Testosterone/urine
3.
Talanta ; 72(4): 1586-92, 2007 Jun 15.
Article in English | MEDLINE | ID: mdl-19071801

ABSTRACT

Composites of hydroxyl-terminated PAMAM dendrimers, generation 4.0 (64 peripheral OH groups) containing either Ir, Pt or Rh nanoparticles were synthesized and characterized in solution. Each one of these composites was then immobilized on a glassy carbon electrode (GC) and incorporated as an amperometric detector for dopamine in a high-performance liquid chromatograph (HPLC). Comparison of the analytical performance of the novel electrochemical detectors with a typical UV-vis optical detector for dopamine revealed that the sensitivity of the GC electrode modified with dendrimer-Rh composite is comparable to that of the spectroscopic detector, with a detection limit of 0.15muM, and is linear up to at least 1.0mM (R(2)=0.998). Furthermore, it was found that the electroanalytical approach suffers minimal matrix effects that arise in the analysis of dopamine in samples of urine.

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