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

被引:19
作者
Sipoli Marques, Marlice Aparecida [1 ]
Gualberto Pereira, Henrique Marcelo [1 ]
Padilha, Monica Costa [1 ]
de Aquino Neto, Francisco Radler [1 ]
机构
[1] Univ Fed Rio de Janeiro, Inst Quim, LAB DOP, LADETEC, BR-21949900 Rio De Janeiro, Brazil
关键词
tetrahydrogestrinone; gestrinone; trenbolone; derivatization;
D O I
10.1016/j.chroma.2006.08.032
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
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. (C) 2006 Elsevier B.V. All rights reserved.
引用
收藏
页码:215 / 225
页数:11
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