Manaf, Normaliza Abdul
(2018)
Development Of New Analytical Methods For Steroid Profiling For Doping Purposes.
PhD thesis, Universiti Sains Malaysia.
Abstract
The steroid profile compounds namely testosterone (T), epitestosterone (E), androsterone (A), etiocholanolone (Etio), 5alpha-androstane-3alpha,17beta-diol (5αAdiol), 5beta-androstane-3alpha,17beta-diol (5βAdiol) and the ratio of T to E (T/E)) has been determined in urine of male volunteers who consumed Tongkat Ali (TA) supplement using the solid phase extraction (SPE) and liquid-liquid extraction (LLE) method. From 47 samples, 11 samples violated the World Anti-Doping Agency (WADA) guidelines and confirmation by gas chromatography combustion isotope ratio mass spectrometry (GC-C-IRMS) showed 5 samples were consistent with the exogenous origin (Δδ13C > 3‰). Two microextraction methods, i.e., vortexassisted liquid-liquid microextraction (VALLME) and micro-solid phase extraction (μ-SPE) followed by LC-MS/MS were developed. Hypersil Gold C18 column (50 mm × 2.1 mm, 1.9 μm) with gradient elution resulted in baseline separation for compounds in about 8 min.
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