Functional pairing between cellular glycoconjugates and tissue lectins like galectins has wide (patho)physiological significance. Their study is facilitated by nonhydrolysable derivatives of the natural O‐glycans, such as S‐ and Se‐glycosides. The latter enable extensive analyses by specific ⁷⁷Se NMR spectroscopy, but still remain underexplored. By using the example of selenodigalactoside (SeDG) and the human galectin‐1 and ‐3, we have evaluated diverse ⁷⁷Se NMR detection methods and propose selective ¹H,⁷⁷Se heteronuclear Hartmann–Hahn transfer for efficient use in competitive NMR screening against a selenoglycoside spy ligand. By fluorescence anisotropy, circular dichroism, and isothermal titration calorimetry (ITC), we show that the affinity and thermodynamics of SeDG binding by galectins are similar to thiodigalactoside (TDG) and N‐acetyllactosamine (LacNAc), confirming that Se substitution has no major impact. ITC data in D₂O versus H₂O are similar for TDG and LacNAc binding by both galectins, but a solvent effect, indicating solvent rearrangement at the binding site, is hinted at for SeDG and clearly observed for LacNAc dimers with extended chain length.

中文翻译：

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Galectin-聚糖相互作用：通过77Se NMR光谱和溶剂（H2O / D2O）对结合的影响进行监测的指南。

细胞糖缀合物和组织凝集素（如半乳凝素）之间的功能配对具有广泛的（病理）生理学意义。天然O-糖苷的不可水解衍生物（例如S-和Se-糖苷）促进了他们的研究。后者可以通过特定的⁷⁷ Se NMR光谱进行广泛的分析，但仍未得到充分开发。通过使用硒二半乳糖苷（SeDG）和人半乳糖凝集素-1和-3的实例，我们评估了多种⁷⁷ Se NMR检测方法，并提出了选择性¹ H，⁷⁷Se异核Hartmann-Hahn转移可有效用于针对硒代糖苷间谍配体的竞争NMR筛选。通过荧光各向异性，圆二色性和等温滴定热法（ITC），我们显示了半乳糖凝集素结合SeDG的亲和力和热力学类似于硫代双糖苷（TDG）和N-乙酰基乳糖胺（LacNAc），证实了Se取代没有主要影响。对于DDG和LacNAc的两种半乳糖凝集素结合，D ₂ O与H ₂ O中的ITC数据相似，但是对于SeDG暗示了溶剂作用，表明溶剂在结合位点的重排，对于具有延长链长的LacNAc二聚体清楚地观察到。