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Raics, Maria; Timari, Istvan; Diercks, Tammo; Szilagyi, Laszlo; Gabius, Hans-Joachim; Kover, Katalin E. (2019): Selenoglycosides as Lectin Ligands: Se-77-Edited CPMG-HSQMBC NMR Spectroscopy To Monitor Biomedically Relevant Interactions. In: Chembiochem, Vol. 20, No. 13: pp. 1688-1692
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The fundamental importance of protein-glycan recognition calls for specific and sensitive high-resolution techniques for their detailed analysis. After the introduction of F-19 NMR spectroscopy to study the recognition of fluorinated glycans, a new Se-77 NMR spectroscopy method is presented for complementary studies of selenoglycans with optimised resolution and sensitivity, in which direct NMR spectroscopy detection on Se-77 is replaced by its indirect observation in a 2D H-1,Se-77 HSQMBC spectrum. In contrast to OH/F substitution, O/Se exchange allows the glycosidic bond to be targeted. As an example, selenodigalactoside recognition by three human galectins and a plant toxin is readily indicated by signal attenuation and line broadening in the 2D H-1,Se-77 HSQMBC spectrum, in which CPMG-INEPT long-range transfer ensures maximal detection sensitivity, clean signal phases, and reliable ligand ranking. By monitoring competitive displacement of a selenated spy ligand, the selective Se-77 NMR spectroscopy approach may also be used to screen non-selenated compounds. Finally, H-1,Se-77 CPMG-INEPT transfer allows further NMR sensors of molecular interaction to be combined with the specificity and resolution of Se-77 NMR spectroscopy.