Capillary gas chromatographic separation of bile acid acyl glycosides without thermal decomposition and isomerization

Takashi Iida, Shoujiro Ogawa, Genta Kakiyama, Takaaki Goto, Nariyasu Mano, Junichi Goto, Toshio Nambara

Research output: Contribution to journalArticlepeer-review

4 Citations (Scopus)

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 μm) of 5% phenyl polysilphenylene-siloxane at a column temperature below 280°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 24α-glucosides were always eluted faster than the corresponding 24β-glucosides, which eluted before the corresponding 24β-galactosides. The method could be usefully applied to biosynthetic and metabolic studies of bile acid acyl glycosides in biological materials.

Original languageEnglish
Pages (from-to)171-176
Number of pages6
JournalJournal of Chromatography A
Volume1057
Issue number1-2
DOIs
Publication statusPublished - 2004 Nov 19

Keywords

  • Bile acid acyl glycosides
  • Capillary gas chromatography
  • Glycosidic conjugates of bile acids
  • Narrow-bore short capillary column
  • TFA derivatives

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry
  • Organic Chemistry

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