Department of Inorganic and Analytical Chemistry, University of Debrecen, Debrecen, Hungary.
Department of Organic Chemistry, University of Debrecen, Debrecen, Hungary.
Methods Mol Biol. 2022;2442:105-123. doi: 10.1007/978-1-0716-2055-7_6.
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 H, C, and N offers promising perspectives. Having therefore prepared selenodigalactoside and revealed its bioactivity as galectin ligand, monitoring of its binding by Se NMR spectroscopy at a practical level becomes possible by setting up a 2D H, Se CPMG-HSQBMC experiment including CPMG-INEPT long-range transfer. This first step into applying Se 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 Se-containing β-galactosides and to build on the gained experience with Se by adding F as second sensor in doubly labeled glycosides.
它们作为多功能效应物的新兴特性解释了人们对监测糖结合到半乳糖凝集素以及确定其配体在溶液中的结合态构象的浓厚兴趣。基本上，NMR 光谱学有助于进行相应的实验。为了开发用于这些目的的新方法甚至更好的方法，将可利用的同位素范围扩展到 H、C 和 N 之外，提供了有希望的前景。因此，我们制备了硒半乳糖苷并揭示了它作为半乳糖凝集素配体的生物活性，通过建立包括 CPMG-INEPT 长程转移的 2D H、Se CPMG-HSQBMC 实验，可以在实际水平上通过 Se NMR 光谱监测其结合。这是首次将 Se 用作半乳糖结合传感器的应用，证明了它在化合物混合物中相对于抑制效力进行筛选以及实现复杂表位作图的潜力。已记录的合成碳水化合物化学和 NMR 光谱学的战略组合促使我们考虑使用同位素纯含硒β-半乳糖苷，并在获得的 Se 经验的基础上，通过在双标记糖苷中添加 F 作为第二个传感器来构建。
