A. Kuksis
Apr 1, 1965
Citations
0
Influential Citations
20
Citations
Quality indicators
Journal
Journal of the American Oil Chemists’ Society
Abstract
Methods are reviewed for the preparation, gasliquid chromatographic (GLC) separation, identification, and quantitative estimation of the trifluoroacetyl derivatives of bile acid methyl esters. Of the stationary phases tried (SE-30, QF-1 and XE-60) methylfluoroalkyl silicone (QF-1) was best suited for analysis of the trifluoroacetates. This phase (1–2% QF-1 on 100–120 mesh Gas Chrom P) allowed an orderly resolution of conformational isomers and consistently gave GLC columns (stainless steel tubes, 1/8 in. O.D. × 3 ft) from which the bile acid derivatives could be recovered in high yield. Applications to biological materials are illustrated with bile acid samples from animal biles and from human duodenal drainage and feces. Identifications of the major bile acids made by the GLC of the trifluoroacetates were confirmed by results obtained with bile acid methyl esters and bile acid methyl ester acetates on QF-1 and the other liquid phases investigated. For most mixtures of bile acids, however, it appears that GLC of methyl esters and methyl ester trifluoroacetates on QF-1 is sufficient for a reliable recognition of common bile acids. Overall accuracy of the estimates was of the order of ± 5%, but it varied with the nature and concn of the component.