Abstract
Methods for the analysis and isolation of heptakis(2,6-di-O-methyl)-β-cyclodextrin (CD) by thin-layer and high-performance liquid chromatography (HPLC) were investigated. By using these methods a commercial and two synthetic samples of heptakis(2,6-di-O-methyl)-β-CD were analysed and it was found that they contained two major and at least four minor components, of which the two major and one minor components were isolated by semi-preparative HPLC. Careful fragmentation analyses, which consisted of successive hydrolysis, reduction, acetylation and characterization of the partially methylated d-glucitol peracetates by gas chromatography—mass spectrometry and determination of molecular weights by fast-atom bombardment mass spectrometry indicated that these compounds were heptakis(2,6-di-O-methyl)-β-CD, hexakis(2,6-di-O-methyl)-mono(2,3,6-tri-O-methyl)-β-CD and pentakis(2,6-di-O-methyl)-bis(2,3,6-tri-O-methyl)-β-CD.
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