Université de Reims Champagne-Ardenne, CNRS, ICMR UMR 7312, 51097 Reims, France.
Analyst. 2021 Sep 7;146(17):5316-5325. doi: 10.1039/d1an00899d. Epub 2021 Aug 2.
The analysis of small molecules within complex mixtures is a particularly difficult task when dealing with the study of metabolite mixtures or chemical reaction media. This issue has fostered in recent years an active search for effective and practical solutions. In this context, the ViscY NMR approach has been recently proposed. ViscY collectively designates the NMR experiments that take advantage of spin diffusion in highly viscous solvents or solvent blends for the individualization of the NMR spectra of small molecule mixture components. Two viscous media were prepared from ortho-phosphoric acid (85%) solution by dilution with either DO or DMSO-d, thus providing solvent blends with slightly different polarities in which all liquid-state NMR experiments can be carried out easily. Two mixtures, one of four structurally close dipeptides and one of four low-polarity phosphorus-containing compounds, were used for the method assessment, using ViscY experiments such as homonuclear selective 1D and 2D H NOESY experiments, heteronuclear 2D H-N/H-P HSQC-NOESY and H-C/H-N/H-P NOAH experiments.
分析复杂混合物中的小分子是一项特别具有挑战性的任务，尤其是在研究代谢物混合物或化学反应介质时。近年来，这一问题促使人们积极寻求有效和实用的解决方案。在这种背景下，ViscY NMR 方法最近被提出。ViscY 是指利用高粘性溶剂或溶剂混合物中的自旋扩散来实现小分子混合物成分的 NMR 谱个体识别的 NMR 实验的统称。通过用 DO 或 DMSO-d 稀释 85%的原磷酸溶液，制备了两种粘性介质，从而提供了极性略有不同的溶剂混合物，其中可以轻松进行所有液态 NMR 实验。使用 ViscY 实验，如同核选择性 1D 和 2D H NOESY 实验、异核 2D H-N/H-P HSQC-NOESY 和 H-C/H-N/H-P NOAH 实验，对两种混合物（四个结构相近的二肽混合物和四个低极性含磷化合物混合物）进行了方法评估。
