ANALYSIS OF CHARGED CYCLOMALTOOLIGOSACCHARIDES (CYCLODEXTRIN) DERIVATIVES BY ION-SPRAY, MATRIX-ASSISTED LASER-DESORPTION IONIZATION TIME-OF-FLIGHT AND FAST-ATOM-BOMBARDMENT MASS-SPECTROMETRY, AND BY CAPILLARY ELECTROPHORESIS/

The use of electrospray-ionization mass spectrometry (ESIMS), matrix-a ssisted laser-desorption/ionization time-of-flight mass spectrometry ( MALDITOFMS), and fast-atom bombardment mass spectrometry (FABMS) for t he rapid determination of molecular weight, degree of substitution (ds ), and purity is demonstrated for charged derivatives of cyclomalto-he ptaose (beta CD) and -octaose (gamma CD). The access to anionic sulfoa lkyl ethers (alkyl: ethyl, n-propyl, and n-butyl) and to beta CD-2-hyd roxy-3-trimethylammoniumpropyl ether chlorides (HTAP-beta CD) leads on ly to mixtures of products, the compositions of which can be determine d directly from ESI and MALDITOF mass spectra. All charged derivatives consist of a mixture of unreacted and higher substituted compounds. T he substitution patterns obtained by MS are in good agreement with the results of experiments on the separation of beta CD-sulfoalkyl ethers by capillary electrophoresis (CE). (C) 1996 Elsevier Science Ltd.