1H HR/MAS NMR in the suspended state: molecular recognition processes in liquid chromatography between steroids and a silica hydride-based cholesterol phase.
1H HR/MAS NMR in the suspended state: molecular recognition processes in liquid chromatography between steroids and a silica hydride-based cholesterol phase.
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悬浮状态下的 1H HR/MAS NMR：液相色谱中类固醇和基于二氧化硅的胆固醇相之间的分子识别过程。
DOI：
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发表时间：
2009
影响因子：
3.1
通讯作者：
K. Albert
中科院分区：
文献类型：
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作者：
V. Friebolin;Marc P Bayer;M. Matyska;J. Pesek;K. Albert
用胆固醇10-十一烷酸酯修饰的硅胶固定相分离了8种甾体化合物的混合物。在类固醇混合物中，孕酮显示出最长的保留时间，表明与固定相材料的相互作用最强。为了获得更详细的信息，有效的分离过程中，相互作用的研究进行了高分辨率/魔角旋转（HR/MAS）NMR光谱记录在悬浮状态。(1)H具有T（1 ρ）抑制的饱和转移差（STD）NMR实验显示孕酮对胆固醇柱材料具有显著的疏水结合亲和力。这些NMR结果可以直接与HPLC获得的色谱数据相关。
A mixture of eight steroids was separated by HPLC on a silica hydride-based stationary phase modified with a moiety of cholesteryl 10-undecanoate. Within the steroid mixture progesterone showed the longest retention time suggesting the strongest interaction with the stationary phase material. To obtain more detailed information upon the effective separation process, interaction studies were performed by high resolution/magic angle spinning (HR/MAS) NMR spectroscopy recorded in the suspended state. (1)H saturation transfer difference (STD) NMR experiments with T(1rho) suppression showed significant hydrophobic binding affinities of progesterone toward the cholesterol column material. These NMR results can be correlated directly to the chromatographic data obtained by HPLC.