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首页> 外文期刊>Proceedings of the National Academy of Sciences of the United States of America >Enhanced diffusion-edited NMR spectroscopy of mixtures using chromatographic stationary phases.
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Enhanced diffusion-edited NMR spectroscopy of mixtures using chromatographic stationary phases.

机译:使用色谱固定相对混合物进行增强的扩散编辑NMR光谱分析。

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摘要

We introduce an analytical method that combines in one pot the advantages of column chromatography separation and NMR structural analysis. The separation of the NMR spectra of the components of a mixture can be achieved according to their apparent diffusion rates [James, T. L. and McDonald, G. G. (1973) J. Magn. Reson. 58, 58-61]. We show that the separation of the spectral components, corresponding to single molecular species, can be enhanced by order of magnitudes upon addition of a typical stationary phase used in HPLC. The solid phase imbibed by the mixture for analysis is an heterogeneous ensemble, so that solid-state NMR methods (high-resolution magic angle spinning) are necessary to recover high-resolution spectra. We demonstrate applications of this combination of high-resolution magic angle spinning and NMR diffusometry on test mixtures for direct (silica gel) and inverse (C18) columns. However, many common chromatographic supports available for HPLC should be readily adaptable for use with this technique.
机译:我们介绍了一种结合了柱色谱分离和NMR结构分析优势的分析方法。混合物的组分的NMR光谱的分离可以根据它们的表观扩散速率来实现[James,T.L。和McDonald,G.G。(1973)J.Magn.Chem.Soc。,1993,9,1959]。雷森58、58-61]。我们显示,在添加用于HPLC的典型固定相后,可以将光谱成分的分离(对应于单个分子种类)提高一个数量级。混合物吸收的用于分析的固相是非均相的,因此固态NMR方法(高分辨率幻角旋转)对于恢复高分辨率光谱是必需的。我们演示了高分辨率魔角旋转和NMR扩散法在直接(硅胶)和反向(C18)色谱柱的测试混合物上的组合应用。但是,许多可用于HPLC的常用色谱支持物应易于适应于该技术。

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