Sialo-CEST: Chemical exchange saturation transfer NMR of oligo- and poly-sialic acids and the assignment of their hydroxyl groups using selective- and HSQC-TOCSY

Hadassah Shinar, Marcos D. Battistel, Michael Mandler, Flora Lichaa, Darón I. Freedberg, Gil Navon

Research output: Contribution to journalArticlepeer-review

Abstract

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, α-2,8 polysialic acid in aqueous solution, yield very significant CEST effects even at 37 °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 1H-1H TOCSY methods or 1H-13C 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.

Original languageEnglish
Pages (from-to)165-173
Number of pages9
JournalCarbohydrate Research
Volume389
Issue number1
DOIs
StatePublished - 7 May 2014

Keywords

  • Chemical exchange saturation transfer (CEST)
  • Exchange rate constants
  • Hydroxyl groups assignments
  • NMR
  • Polysialic acid
  • Sialic acid

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