Purification and analysis of partially alkylated cyclodextrins by liquid and gas chromatography
- 1 October 1993
- journal article
- research article
- Published by Wiley in Journal of High Resolution Chromatography
- Vol. 16 (10), 587-593
- https://doi.org/10.1002/jhrc.1240161004
Abstract
Complex mixtures of partially alkylated cyclodextrins can be analyzed by both HPLC and high temperature capillary GC. Because of the limited efficiency of LC, suitable analytical and preparative separations can be achieved only with systems of carefully optimized selectivity. Using LC it has been possible to isolate and purify single cyclodextrin species from very complex mixtures of components which contain unreacted hydroxyl groups in addition to the alkoxy groups. Analysis of the reaction mixtures and of fractions taken from LC separations can be performed with advantage by high resolution capillary GC at high temperatures between 300 and 400 °C. The thermal stability of partially alkylated cyclodextrins in high temperature GC is considerably increased by trimethylsilylation of the free hydroxyl groups. Fast atom bombardment mass spectrometry and proton NMR were used to identify species isolated from the preparative LC separations.Keywords
This publication has 7 references indexed in Scilit:
- Molecular modelling experiments on chiral recognition in GC with specially derivatized cyclodextrins as selectorsJournal of High Resolution Chromatography, 1993
- Preparation, purification, and analysis of alkylated cyclodextrinsJournal of High Resolution Chromatography, 1992
- Isolation and characterization of heptakis(2,6-di-O-methyl)cyclomaltoheptaose and over-methylated homologuesCarbohydrate Research, 1989
- Analysis of heptakis(2,6-di-O-methyl)-β-cyclodextrin by thin-layer, high-performance liquid and gas chromatography and mass spectrometryJournal of Chromatography A, 1986
- Syntheses of stationary phases for reversed-phase LC using silanization and polymer coatingChromatographia, 1984
- Immobilization of stationary liquids in reversed- and normal-phase liquid chromatography : Production and testing of materials for bonded-phase chromatographyJournal of Chromatography A, 1983
- Cyclodextrin chemistry. Selective modification of all primary hydroxyl groups of α‐ and β‐cyclodextrinsHelvetica Chimica Acta, 1978