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Characterization of Metallosupramolecular Polymers by Top‐Down Multidimensional Mass Spectrometry Methods
Author(s) -
Guo Kai,
Guo Zaihong,
Ludlow James M.,
Xie Tingzheng,
Liao Shengyun,
Newkome George R.,
Wesdemiotis Chrys
Publication year - 2015
Publication title -
macromolecular rapid communications
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.348
H-Index - 154
eISSN - 1521-3927
pISSN - 1022-1336
DOI - 10.1002/marc.201500084
Subject(s) - mass spectrometry , ion mobility spectrometry , electrospray ionization , supramolecular chemistry , chemistry , characterization (materials science) , ion , polymer , tandem mass spectrometry , ion mobility spectrometry–mass spectrometry , analytical chemistry (journal) , materials science , chemical physics , nanotechnology , sample preparation in mass spectrometry , molecule , organic chemistry , chromatography
Top‐down multidimensional mass spectrometry, interfacing electrospray ionization (ESI) with ion mobility mass spectrometry (IM‐MS), and energy resolved (gradient) tandem mass spectrometry (gMS 2 ) are employed to characterize the stoichiometries, architectures, and intrinsic stabilities of coordinatively bound supramolecular polymers containing terpyridine functionalized ligands. As a soft ionization method, ESI prevents or minimizes unwanted assembly destruction. The IM dimension affords separation of the supramolecular ions by charge and collision cross‐section (a function of size and shape). The mobility separated ions are subsequently identified by their mass‐to‐charge‐ratios and isotope patterns in the orthogonal MS dimension. Finally, the gMS 2 dimension reveals bond breaking proclivities and disintegration pathways of the assemblies. The described methodology does not require high sample purity due to the dispersive nature of the IM and MS steps. Its utility is demonstrated with the comprehensive analysis of bisterpyridine‐based metallomacrocycle mixtures and a tristerpyridine based complex with 3‐D nanosphere‐like architecture.