Polysulfated Carbohydrates Analyzed as Ion-Paired Complexes with Basic Peptides and Proteins Using Electrospray Negative Ionization Mass Spectrometry

Siegel, Marshall M.
Tabei, Keiko
Kagan, Michael Z.
Vlahov, Ioncho R.
Hileman, Ronald E.
Linhardt, Robert J.
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Biology , Chemistry and chemical biology , Chemical and biological engineering , Biomedical engineering
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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.
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.
Journal of Mass Spectrometry, 32, 760-772
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The Linhardt Research Labs.
The Shirley Ann Jackson, Ph.D. Center for Biotechnology and Interdisciplinary Studies (CBIS)
The Linhardt Research Labs Online Collection
Rensselaer Polytechnic Institute, Troy, NY
Journal of Mass Spectrometry