Abstract
Their emerging nature as multifunctional effectors explains the large interest to monitor glycan binding to galectins and to define bound-state conformer(s) of their ligands in solution. Basically, NMR spectroscopy facilitates respective experiments. Towards developing new and even better approaches for these purposes, extending the range of exploitable isotopes beyond 1H, 13C, and 15N offers promising perspectives. Having therefore prepared selenodigalactoside and revealed its bioactivity as galectin ligand, monitoring of its binding by 77Se NMR spectroscopy at a practical level becomes possible by setting up a 2D 1H, 77Se CPMG-HSQBMC experiment including CPMG-INEPT long-range transfer. This first step into applying 77Se as sensor for galectin binding substantiates its potential for screening relative to inhibitory potencies in compound mixtures and for achieving sophisticated epitope mapping. The documented strategic combination of synthetic carbohydrate chemistry and NMR spectroscopy prompts to envision to work with isotopically pure 77Se-containing β-galactosides and to build on the gained experience with 77Se by adding 19F as second sensor in doubly labeled glycosides.
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Acknowledgments
This research was supported by the National Research, Development and Innovation Office of Hungary (grant numbers: NKFI/OTKA NN 128368) (to M.R., L.Sz., and K.E.K.) and NKFI/OTKA PD 135034 (to I.T.)) and co-financed by the European Regional Development Fund (project GINOP-2.3.2-15-2016-00044). I.T. acknowledges the support of the János Bolyai Research Scholarship of the Hungarian Academy of Sciences (BO/00372/20/7). L.Sz. is indebted to Sára Balla for excellent help in organic syntheses, to Lajos Nagy for MS spectra and to Attila Kiss for optical rotation data (all in the Department of Chemistry, Faculty of Science & Technology, University of Debrecen).
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Raics, M., Timári, I., Szilágyi, L., Gabius, HJ., Kövér, K.E. (2022). Introducing 77Se NMR Spectroscopy to Analyzing Galectin –Ligand Interaction. In: Stowell, S.R., Arthur, C.M., Cummings, R.D. (eds) Galectins. Methods in Molecular Biology, vol 2442. Humana, New York, NY. https://doi.org/10.1007/978-1-0716-2055-7_6
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