Determination of 13C/12C ratios of endogenous urinary steroids : method validation, reference population and implication for doping control purposes

Publikation: Beitrag in Buch/Bericht/KonferenzbandKonferenzbeitrag - Aufsatz in KonferenzbandForschung

Abstract

The application of a comprehensive gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS)-based method for stable carbon isotopes of endogenous urinary steroids is presented. The key element in sample preparation is the consecutive clean up with high performance liquid chromatography (HPLC) of underivatized and acetylated steroids, which allows the isolation of ten analytes (11ß-hydroxy-androsterone, 5α-androst-16-en-3α-ol, pregnanediol, androsterone, etiocholanolone, testosterone, epitestosterone, 5α-androstane-3α, 17ß-diol, 5ß-androstane-3α, 17ß-diol and dehydroepiandrosterone) from a single urine specimen. These steroids are of particular importance to doping controls as they enable the sensitive and retrospective detection of steroid abuse by athletes. Depending on the biological background, the determination limit for all steroids ranges from 5 to 10 ng/mL for a 10 mL specimen. The method is validated by means of linear mixing models for each steroid, which covers the items repeatability and reproducibility. Specificity was further demonstrated by gas chromatography/mass spectrometry (GC/MS) for each analyte, and no influence of the sample preparation or the quantity of analyte on carbon isotope ratios was observed. In order to determine naturally occurring 13C/ 12C ratios of all implemented steroids, a reference population of n = 61 subjects was measured to enable the calculation of reference limits for all relevant steroidal ∆ values. Verf.-Referat
OriginalspracheEnglisch
TitelRecent advances in doping analysis (16) : Proceedings of the Manfred Donike Workshop ; 26th Cologne Workshop on Dope Analysis, 24th to 29th February 2008
Herausgeber*innenWilhelm Schänzer, Hans Geyer, A. Gotzmann, Ute Mareck
Seitenumfang1
Herausgeber (Verlag)Sportverlag Strauß
Erscheinungsdatum2008
Seiten151
PublikationsstatusVeröffentlicht - 2008
VeranstaltungCologne Workshop on Dope Analysis - Köln, Deutschland
Dauer: 24.02.200829.02.2008
Konferenznummer: 26

Fachgebiete und Schlagwörter

  • Biochemie
  • Doping
  • Dopingnachweis
  • Flüssigkeitschromatographie
  • Gaschromatographie
  • Massenspektrometrie
  • Messverfahren
  • Sportmedizin
  • Steroid
  • Untersuchungsmethode
  • Urin
  • Urinausscheidung
  • Validität

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