GC-MS Derivatization Studies: The Formation of Dexamethasone MO-TMS
作者:
J-P. Thenot,
E.C. Horning,
期刊:
Analytical Letters
(Taylor Available online 1972)
卷期:
Volume 5,
issue 12
页码: 905-913
ISSN:0003-2719
年代: 1972
DOI:10.1080/00032717208062155
出版商: Taylor & Francis Group
关键词: gas chromatography;mass spectrometry;dexamethasone;prednisone;prednisolone;methoxime;trimethylsilyl derivative
数据来源: Taylor
摘要:
The 16α-methyl group in dexamethasone increases drastically the steric hindrance to reaction of both the 20-ketone and 17α-hydroxyl groups, as shown by kinetic studies with GC-MS techniques. A procedure is described for the preparation of the MO derivative (reaction et 60[ddot]C for 3 hr) and complete conversion of all hydroxyl groups to TMS ether groups (reaction at 100[ddot]C for 6 hr). The resulting MO-TMS derivative is thermostable and suitable for use in GC-MS methods. The procedures usually employed in urinary steroid studies are satisfactory for prednisone and prednisolone.
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