Analysis of sulfobutyl ether-beta-cyclodextrin mixtures by ion-spray mass spectrometry and liquid chromatography-ion-spray mass spectrometry.
The analysis of two commercial and two home-made sulfobutyl ether beta-cyclodextrin (SBE-beta-CD) samples by ion-spray (IS) mass spectrometry and by liquid chromatography-mass spectrometry coupling (LC-MS) is investigated in a negative ion mode. SBE-beta-CD fragmentation was first investigated by direct infusion. In IS, the best conditions for SBE-beta-CD ionization consisted of ammonium acetate added to an acetonitrile/water mixture as sample solvent. These conditions allowed simplification of the mass spectrum, mainly by the formation of dicharged species [M-2H]2-, thus limiting the production of multicharged fragments. IS-MS permits fast and simple measurement of the substitution pattern and determination of the global degree of substitution for SBE-beta-CD mixtures. A complementary method using LC-MS was developed for the analysis of these mixtures. The substitution patterns obtained by LC-MS are in good agreement with those determined by direct MS analysis. The LC-MS coupling enabled separation of the mixtures versus the charge in anion-exchange chromatography (AEC) whereas no separation of the different substitution isomers potentially present in the SBE-beta-CD mixture was displayed. The AEC methodology described can be successfully used for fractionation of SBE-beta-CD derivatives at the semi-preparative scale.
Grard
S
S
Institut de Chimie Organique et Analytique, ICOA, CNRS-UMR 6005, Université d'Orléans, France.
Elfakir
C
C
Dreux
M
M
D002853:Chromatography, Liquid / Q000379:methods*; D003505:Cyclodextrins / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods*; D047392:beta-Cyclodextrins
D003505:Cyclodextrins; D047392:beta-Cyclodextrins; C093196:SBE4-beta-cyclodextrin