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Abstract
Current tandem mass spectrometry-based methods for cyclodextrin characterization rely on exact mass and fragmentation patterns. In general, orthogonal methods provide additional information, which increases confidence in characterization. Ion mobility spectrometry (IMS) and mass spectrometry (MS) provide two dimensions of analysis based on molecular weight and size. Here, we report new gas phase behavior of sodiated cyclodextrins revealed by Cyclic IMS coupled to tandem MS. Gas phase ion activation prior to IMS separation on sodiated α-, β-, and γ-cyclodextrins generates isomeric species with different mobilities. Fragmentation studies on all isomers following gas phase separation showed a greater degree of fragmentation than was observed for the original sodiated cyclodextrins. These findings suggest that sodiated cyclodextrins undergo structural changes upon activation, with the newly formed isomers significantly contributing to fragmentation. To our knowledge this is the first report on separation of isomeric ions generated upon collisional activation of sodiated cyclodextrins in the gas phase. Results of this study can be used for better understanding of cyclodextrin fragmentation. Additionally, these findings can be used to develop more specific methodologies for cyclodextrin characterization.
Supplementary materials
Title
Main Supporting Information
Description
Mobilogram for sodiated β-cyclodextrin at 5 V trap injection voltage and 5 V transfer injection voltage after one pass, mass spectrum of doubly charged dimer of sodiated β-cyclodextrin, mass spectrum of sodiated β-cyclodextrin, mobilogram of sodiated β-cyclodextrin at 50 V trap injection voltage 5 V transfer injection voltage after one pass, mobilogram of sodiated β-cyclodextrin at 95 V trap injection voltage and 5 V transfer injection voltage after one pass, mobilograms of sodiated β-cyclodextrin at 75 V trap injection voltage and a) 5 V, b) 75 V and c) 80 V transfer injection voltage after one pass through the Cyclic IMS, table for traveling wave parameters, table for cyclic sequence for β-cyclodextrin, table for cyclic sequence for α-cyclodextrin, table for cyclic sequence for γ-cyclodextrin
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Title
Mobilograms of pre-IMS collisional activation
Description
Mobilograms of pre-IMS collisional activation of alpha, beta, and gamma cyclodextrins at varying pre-IMS activation from 5 V to 150 V with an increment of 5 V and constant post-IMS activation of 5 V.
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