Journal
CARBOHYDRATE RESEARCH
Volume 389, Issue -, Pages 165-173Publisher
ELSEVIER SCI LTD
DOI: 10.1016/j.carres.2014.02.008
Keywords
Sialic acid; Polysialic acid; Chemical exchange saturation transfer (CEST); NMR; Exchange rate constants; Hydroxyl groups assignments
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Chemical exchange saturation transfer (CEST) is an NMR method that takes advantage of proton exchange between solute and solvent molecules in dynamic equilibrium, enabling the detection of the solute NMR signals with enhanced sensitivity. Herein, we report that the hydroxyl groups in a naturally occurring polysaccharide, alpha-2,8 polysialic acid in aqueous solution, yield very significant CEST effects even at 37 degrees C where the resonances of the hydroxyl groups are not directly observed. We also report the assignments of the hydroxyl groups for the polymer and its oligomeric building blocks, from monomer to hexamer. We show that the same assignments can be made by either H-1-H-1 TOCSY methods or H-1-C-13 HSQC-TOCSY methods, to alleviate spectral overlap. Finally, we report the exchange rates of the OH groups with water and show how these rates can be used to select and fine-tune CEST effects. (C) 2014 Elsevier Ltd. All rights reserved.
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