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

doi:10.1016/j.chroma.2004.09.029

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

University Hospital (not affiliated with any section)

Research output: Contribution to journal › Article › peer-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 language	English
Pages (from-to)	171-176
Number of pages	6
Journal	Journal of Chromatography A
Volume	1057
Issue number	1-2
DOIs	https://doi.org/10.1016/j.chroma.2004.09.029
Publication status	Published - 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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10.1016/j.chroma.2004.09.029

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Capillary gas chromatographic separation of bile acid acyl glycosides without thermal decomposition and isomerization. / Iida, Takashi; Ogawa, Shoujiro; Kakiyama, Genta; Goto, Takaaki ; Mano, Nariyasu; Goto, Junichi; Nambara, Toshio.

In: Journal of Chromatography A, Vol. 1057, No. 1-2, 19.11.2004, p. 171-176.

Research output: Contribution to journal › Article › peer-review

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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.",

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

author = "Takashi Iida and Shoujiro Ogawa and Genta Kakiyama and Takaaki Goto and Nariyasu Mano and Junichi Goto and Toshio Nambara",

note = "Funding Information: This work was supported in part by a Grant-in-Aid for Scientific Research from the Ministry of Education, Sciences, Sports and Culture of Japan.",

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AU - Iida, Takashi

AU - Ogawa, Shoujiro

AU - Kakiyama, Genta

AU - Goto, Takaaki

AU - Mano, Nariyasu

AU - Goto, Junichi

AU - Nambara, Toshio

N1 - Funding Information: This work was supported in part by a Grant-in-Aid for Scientific Research from the Ministry of Education, Sciences, Sports and Culture of Japan.

PY - 2004/11/19

Y1 - 2004/11/19

N2 - 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.

AB - 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.

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KW - Capillary gas chromatography

KW - Glycosidic conjugates of bile acids

KW - Narrow-bore short capillary column

KW - TFA derivatives

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