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 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.
Marques
Marlice Aparecida Sípoli
MA
LAB DOP-LADETEC, Instituto de Química, Universidade Federal do Rio de Janeiro, Ilha do Fundão, CT, Bloco A, Sala 512, Rio de Janeiro, RJ 21949-900, Brazil.
Pereira
Henrique Marcelo Gualberto
HM
Padilha
Monica Costa
MC
de Aquino Neto
Francisco Radler
FR
D000328:Adult; D005260:Female; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D005867:Gestrinone / Q000031:analogs & derivatives* / Q000032:analysis / Q000737:chemistry / Q000652:urine*; D006801:Humans; D015394:Molecular Structure; D015203:Reproducibility of Results; D014204:Trenbolone Acetate / Q000032:analysis / Q000737:chemistry / Q000652:urine*
D005867:Gestrinone; C479553:tetrahydrogestrinone; D014204:Trenbolone Acetate