Analysis of synthetic 19-norsteroids trenbolone, tetrahydrogestrinone and gestrinone by gas chromatography–mass spectrometry

Tetrahydrogestrinone, gestrinone and trenbolone are synthetic 19-norsteroids with androgenic properties sharing a labile conjugated ketotrienyl motif. Their LC–MS analyses tend to overcome classical derivatization problems, a shortcoming to the use of GC–MS. Therefore, alternative derivatization pro...

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Bibliographic Details
Published in:Journal of Chromatography A 2007-05, Vol.1150 (1), p.215-225
Main Authors: Marques, Marlice Aparecida Sípoli, Pereira, Henrique Marcelo Gualberto, Padilha, Monica Costa, de Aquino Neto, Francisco Radler
Format: Article
Language:English
Subjects:
Adult
Analysis
Biological and medical sciences
Derivatization
Female
Gas Chromatography-Mass Spectrometry - methods
General pharmacology
Gestrinone
Gestrinone - analogs & derivatives
Gestrinone - analysis
Gestrinone - chemistry
Gestrinone - urine
Humans
Medical sciences
Molecular Structure
Pharmacology. Drug treatments
Reproducibility of Results
Tetrahydrogestrinone
Trenbolone
Trenbolone Acetate - analysis
Trenbolone Acetate - chemistry
Trenbolone Acetate - urine
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Summary:Tetrahydrogestrinone, gestrinone and trenbolone are synthetic 19-norsteroids with androgenic properties sharing a labile conjugated ketotrienyl motif. Their LC–MS analyses tend to overcome classical derivatization problems, a shortcoming to the use of GC–MS. Therefore, alternative derivatization procedures were evaluated. The procedure with methoxylamine: pyridine followed by TMSImid: MSTFA gave the best results. This is attributed to the stability of the MO-TMS derivatives hindering the formation of artifacts and tautomerism. A full method is presented including SPE, hydrolysis and liquid–liquid extraction. It was possible to confirm the analytes below 2 ng/mL in urine, being the method robust and cost effective also for screening proposes.
ISSN:0021-9673
DOI:10.1016/j.chroma.2006.08.032