Analysis of synthetic 19-norsteroids trenbolone, tetrahydrogestrinone and gestrinone by gas chromatography-mass spectrometry |
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Authors: | Marques Marlice Aparecida Sípoli Pereira Henrique Marcelo Gualberto Padilha Monica Costa de Aquino Neto Francisco Radler |
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Affiliation: | Department of Analytical Chemistry, University of Seville, C/Profesor Garcia González no 1, 41012 Seville, Spain. agonzale@us.es |
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Abstract: | 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. |
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