Structurally informative tandem mass spectrometry of highly sulfated natural and chemo-enzymatically synthesized heparin and heparan sulfate glycosaminoglycans

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Authors
Kailemia, M.J.
Li, L.
Xu, Y.
Liu, J.
Linhardt, Robert J.
Amster, I.J.
Issue Date
2013
Type
Article
Language
en_US
Keywords
Biology , Chemistry and chemical biology , Chemical and biological engineering , Biomedical engineering
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Abstract
The highly sulfated glycosaminoglycan oligosaccharides derived from heparin and heparan sulfate have been a highly intractable class of molecules to analyze by tandem mass spectrometry. Under the many methods of ion activation, this class of molecules generally exhibits SO3 loss as the most significant fragmentation pathway, interfering with the assignment of the location of sulfo groups in glycosaminoglycan chains. We report here a method that stabilizes sulfo groups and facilitates the complete structural analysis of densely sulfated (two or more sulfo groups per disaccharide repeat unit) heparin and heparan sulfate oligomers. This is achieved by complete removal of all ionizable protons, either by charging during electrospray ionization or by Na+/H+ exchange. The addition of millimolar levels of NaOH to the sample solution facilitates the production of precursor ions that meet this criterion. This approach is found to work for a variety of heparin sulfate oligosaccharides derived from natural sources or produced by chemoenzymatic synthesis, with up to 12 saccharide subunits and up to 11 sulfo groups.
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Molecular and Cellular Proteomics, 12, 979-90
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Full Citation
Structurally informative tandem mass spectrometry of highly sulfated natural and chemo-enzymatically synthesized heparin and heparan sulfate glycosaminoglycans, M. J. Kailemia, L. Li, Y. Xu, J. Liu, R. J. Linhardt, I. J. Amster, Molecular and Cellular Proteomics, 12, 979-90, 2013.
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Elsevier
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