title: Capillary gas chromatographic separation of bile acid acyl glycosides without thermal decomposition and isomerization.
abstract: A direct method for the capillary gas chromatographic (cGC) separation of the acyl glycosides of bile acids was successfully attained. The free acyl glycosides were derivatized to their complete trifluoroacetyl (TFA) derivatives with N-methyl-bis(trifluoroacetamide). The highly volatile TFA derivatives were chromatographed on a short-length (10 m), narrow-bore (0.1 mm) capillary column coated with a thin film (0.1 microm) of 5% phenyl polysilphenylene-siloxane at a column temperature below 280 degrees C. Each exhibited a single, well-separated peak of the theoretical shape without any accompanying peaks due to the thermal decomposition and isomerization. The bile acid 24alpha-glucosides were always eluted faster than the corresponding 24beta-glucosides, which eluted before the corresponding 24beta-galactosides. The method could be usefully applied to biosynthetic and metabolic studies of bile acid acyl glycosides in biological materials.
authors.affiliation: Department of Chemistry, College of Humanities and Sciences, Nihon University, Sakurajousui, Setagaya, Tokyo 156-8550, Japan. takaiida@chs.nihon-u.ac.jp
authors.forename: Takashi
authors.initials: T
authors.lastname: Iida
authors.forename: Shoujiro
authors.initials: S
authors.lastname: Ogawa
authors.forename: Genta
authors.initials: G
authors.lastname: Kakiyama
authors.forename: Takaaki
authors.initials: T
authors.lastname: Goto
authors.forename: Nariyasu
authors.initials: N
authors.lastname: Mano
authors.forename: Junichi
authors.initials: J
authors.lastname: Goto
authors.forename: Toshio
authors.initials: T
authors.lastname: Nambara
mesh_terms: D001647:Bile Acids and Salts / Q000302:isolation & purification*; D002849:Chromatography, Gas / Q000379:methods*; D006027:Glycosides / Q000302:isolation & purification*; D006358:Hot Temperature; D007536:Isomerism; D021241:Spectrometry, Mass, Electrospray Ionization
chemical_list: D001647:Bile Acids and Salts; D006027:Glycosides