Development of an analytical method for the determination of the misuse in sports of boldenone through the analysis of urine by on-line coupling liquid chromatography-gas chromatography-combustion-isotope ratio mass spectrometry.
J Chromatogr A
; 1370: 171-8, 2014 Nov 28.
Article
en En
| MEDLINE
| ID: mdl-25454142
ABSTRACT
Boldenone (Bo), androsta-1,4-dien-17ß-ol-3-one, is an anabolic androgenic steroid not clinically approved for human application. Despite this, many cases are reported every year of athletes testing positive for Bo or its main metabolite 5ß-androst-1-en-17ß-ol-3-one (BoM). Recently the capability of different human intestinal bacteria to produce enzymes able to modify endogenous steroids in Bo has been demonstrated. When a urinary concentration of Bo and/or BoM between 5 and 30 ng/mL is measured a complementary analysis by gas chromatography combustion isotope ratio mass spectrometry (GC-C-IRMS) must be carried out to discriminate the endogenous or exogenous origin. In the present work, a novel analytical method that couples LC-GC by means of the TOTAD interface with C-IRMS is described. The method is based on a first RPLC separation of unacetyled steroids, followed by acetylation and automated on-line LC-GC-C-IRMS, which includes a second RPLC clean-up of acetyl Bo and BoM, isolation of the two fractions in a fraction collector and their consecutive analysis by GC-C-IRMS. The method has been applied to the analysis of urine samples fortified at 5 and 10 ng/mL, where it has shown a good performance.
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MEDLINE
Asunto principal:
Testosterona
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Cromatografía Líquida de Alta Presión
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Anabolizantes
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Cromatografía de Gases y Espectrometría de Masas
Idioma:
En
Revista:
J Chromatogr A
Año:
2014
Tipo del documento:
Article