University of Tuebingen, Institute of Organic Chemistry, Auf der Morgenstelle 18, 72076 Tuebingen, Germany.
Magn Reson Chem. 2010 Feb;48(2):111-6. doi: 10.1002/mrc.2551.
In the current work a racemate of (R)- and (S)-benzylmandelate was separated with a stereoselective polysaccharide-based chiral stationary phase by HPLC. To elucidate the occurring chiral molecular recognition processes in the heterogeneous system used, NMR spectroscopy was chosen under high resolution/magic angle spinning (HR/MAS) NMR conditions in the suspended state. Therefore, and as a proof of concept, a combination of several NMR methods such as spin-lattice relaxation time (T(1)) measurements (T(1)), the saturation transfer difference, and the 2D experiment of the transferred nuclear overhauser enhancement spectroscopy technique were applied. With HR/MAS NMR it is feasible to combine NMR and chromatography to achieve further insights into the separation process.
在目前的工作中，（R）-和（S）-苄基扁桃酸盐的外消旋混合物通过 HPLC 用手性多糖固定相进行了分离。为了阐明在使用的非均相体系中发生的手性分子识别过程，在悬浮状态下选择高分辨率/魔角旋转（HR/MAS）NMR 条件下的 NMR 光谱。因此，作为概念验证，应用了几种 NMR 方法的组合，例如自旋晶格弛豫时间（T（1））测量（T（1））、饱和转移差和转移核 Overhauser 增强光谱技术的二维实验。通过 HR/MAS NMR，可以将 NMR 和色谱结合起来，进一步深入了解分离过程。
