TY - JOUR
T1 - Capillary gas chromatographic separation of bile acid acyl glycosides without thermal decomposition and isomerization
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.
KW - Bile acid acyl glycosides
KW - Capillary gas chromatography
KW - Glycosidic conjugates of bile acids
KW - Narrow-bore short capillary column
KW - TFA derivatives
UR - http://www.scopus.com/inward/record.url?scp=7744227210&partnerID=8YFLogxK
UR - http://www.scopus.com/inward/citedby.url?scp=7744227210&partnerID=8YFLogxK
U2 - 10.1016/j.chroma.2004.09.029
DO - 10.1016/j.chroma.2004.09.029
M3 - Article
C2 - 15584236
AN - SCOPUS:7744227210
VL - 1057
SP - 171
EP - 176
JO - Journal of Chromatography A
JF - Journal of Chromatography A
SN - 0021-9673
IS - 1-2
ER -