Abstract
Methylation of β-cyclodextrin (β-CD, cyclomaltoheptaose) gave under basic conditions a complicated mixture containing 16 partially methylated products. Thus the components were separated by repeated chromatography. Various matrices were examined to obtain intense signals of their molecular ion species under FABMS conditions, and m-nitrobenzylalcohol was found to be the most suitable matrix. In order to determine the structures of the three positional isomers of partially methylated β-CDs (1, 2 and 3) with the nominal molecular weight 1358 and abbreviated as 5D2T-β-CD, the fragmentation based on the cleavage of the glycosidic bonds were carefully examined by B/E-constant linked scanning and tandem mass spectrometry.