在旋转蔗糖溶液和琼脂糖凝胶中自旋扩散条件下通过NMR进行极性混合物分析,Faraday Discussions

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在旋转蔗糖溶液和琼脂糖凝胶中自旋扩散条件下通过NMR进行极性混合物分析
Faraday Discussions ( IF 3.3 ) Pub Date : 2018-12-17 , DOI: 10.1039/c8fd00226f
Pedro Lameiras _{1,

2,

3,

4,

5} , Simon Mougeolle _{1,

2,

3,

4,

5} , François Pedinielli _{1,

2,

3,

4,

5} , Jean-Marc Nuzillard _{1,

2,

3,

4,

5}

Affiliation

首次报道了使用两种新的粘性溶剂，蔗糖溶液和琼脂糖凝胶，以获取混合物中极性和潜在生物活性化合物的单个NMR光谱。在粘性条件下，中小分子在溶液中的翻转速率降低，因此纵向交叉松弛促进了自旋扩散的观察。其结果是，所有的共振¹同一分子内的H核倾向于在2D NOESY光谱中相互关联，从而为进行混合物分析铺平了道路。这项工作描述了通过在同核选择性1D NOESY，选择性2D中自旋扩散而溶解在蔗糖溶液和琼脂糖凝胶各自中的四个结构紧密混合的二肽的个体化：Leu-Val，Leu-Tyr，Gly-Tyr和Ala-Tyr。 NOESY实验和异核2D HSQC-NOESY。蔗糖溶液应优先于琼脂糖凝胶进行研究，以研究由小而柔软的极性化合物制成的混合物，因为琼脂糖凝胶具有产生不提供浓稠的好处，因为它能够产生更合适的粘性条件，从而有效地进行自旋扩散由于有效的横向弛豫，残留的溶剂质子信号。

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Polar mixture analysis by NMR under spin diffusion conditions in viscous sucrose solution and agarose gel

The use of two new viscous solvents, sucrose solution and agarose gel, is reported for the first time for giving access to the individual NMR spectra of polar and potentially bioactive compounds in a mixture. Under viscous conditions, the tumbling rate of small and mid-sized molecules reduces in solution, so that the longitudinal cross-relaxation encourages the observation of spin diffusion. As a result, all of the resonances of the ¹H nuclei within the same molecule tend to correlate together in a 2D NOESY spectrum, thus paving the way to mixture analysis. This work describes the individualization of four structurally close mixed dipeptides: Leu–Val, Leu–Tyr, Gly–Tyr and Ala–Tyr dissolved in each of sucrose solution and agarose gel, by means of spin diffusion in homonuclear selective 1D NOESY, selective 2D NOESY experiments and heteronuclear 2D HSQC-NOESY. Sucrose solution should be preferred to agarose gel for the investigation of mixtures made of small and flexible polar compounds, due to its capability to give rise to more suitable viscous conditions mandatory for efficient spin diffusion, even though agarose gel reveals the benefit of not offering intense residual solvent proton signals due to active transverse relaxation.

更新日期：2019-08-15

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