Polysulfated Carbohydrates Analyzed as Ion-Paired Complexes with Basic Peptides and Proteins Using Electrospray Negative Ionization Mass Spectrometry
No Thumbnail Available
Authors
Siegel, Marshall M.
Tabei, Keiko
Kagan, Michael Z.
Vlahov, Ioncho R.
Hileman, Ronald E.
Linhardt, Robert J.
Issue Date
1997-07-01
Type
Article
Language
ENG
Keywords
Biology , Chemistry and chemical biology , Chemical and biological engineering , Biomedical engineering
Alternative Title
Abstract
Electrospray ionization mass spectrometry was used in the negative ion mode to analyze complexes of sucrose octasulfate, sucrose heptasulfate and sulfated alpha-, beta- and gamma-cyclodextrins with synthetically prepared basic peptides, the basic protein ubiquitin and polyamines. The spectra presented demonstrate that complexes with these basic molecules facilitate the analysis of these polysulfated oligosaccharides. Stable (1:1) complexes result from the ion pairing between the protonated basic arginine and lysine residues of the peptide and the anionic sulfate groups of the polysulfated oligosaccharides. Fragmentation of the polysulfated oligosaccharides resulting in the loss of SO3 could be suppressed by controlling the experimental conditions, such as the nozzle-skimmer voltage, used to obtain the spectra. In the absence of fragmentation, it was possible to obtain data on the purity of sucrose octasulfate and sucrose heptasulfate as well as the distribution of the sulfated cyclodextrins. The confounding presence of sodium counter-ions is also eliminated using this method. Complete chemical sulfation of oligosaccharides is difficult to achieve. Thus, data on sample purity are essential for the characterization of sulfated oligosaccharides used as pharmaceutical agents.
Description
Journal of Mass Spectrometry, 32, 760-772
Note : if this item contains full text it may be a preprint, author manuscript, or a Gold OA copy that permits redistribution with a license such as CC BY. The final version is available through the publisher’s platform.
Note : if this item contains full text it may be a preprint, author manuscript, or a Gold OA copy that permits redistribution with a license such as CC BY. The final version is available through the publisher’s platform.
Full Citation
Polysulfated Carbohydrates Analyzed as Ion-Paired Complexes withBasic Peptides and Proteins Using Electrospray Negative Ionization MassSpectrometry, Marshall M. Siegel, Kieko Tabei, M. Z. Kagan, I. R. Vlahov,R. E. Hileman, R.J. Linhardt, Journal of Mass Spectrometry, 32,760-772, 1997.
Publisher
Terms of Use
Journal
Volume
Issue
PubMed ID
DOI
ISSN
10765174