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Derivatization of 5α‐cholestane‐3β,5,6β‐triol into trimethylsilyl ether sterol for GC analysis
Author(s) -
Park Peter S. W.,
Addis Paul B.
Publication year - 1989
Publication title -
journal of the american oil chemists' society
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.512
H-Index - 117
eISSN - 1558-9331
pISSN - 0003-021X
DOI - 10.1007/bf02636192
Subject(s) - derivatization , trimethylsilyl , triol , chemistry , ether , gas chromatography–mass spectrometry , gas chromatography , derivative (finance) , mass spectrometry , chromatography , nuclear magnetic resonance spectroscopy , organic chemistry , diol , financial economics , economics
Chemical identity of 5α‐cholestane‐3β,5,6β‐triol (C‐Triol) as a trimethylsilyl (TMS) ether derivative was studied using gas chromatography (GC), mass spectrometry (MS), and proton nuclear magnetic resonance (NMR) spectroscopy. The derivatization mixture, held at 23°C for 30 and 300 min, showed only a single peak (B) by GC. When the mixture was heated at 70°C for a few hours, another peak (A) emerged ahead of peak (B). GC‐MS analysis revealed that the GC peaks (A) and (B) are C‐Triol as tris ‐ and bis ‐TMS ether derivatives, respectively. NMR analysis suggested that the hydroxyl groups at C 3 and C 6 of C‐Triol were involved in the formation of the bis ‐TMS ether.