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使用高效液相色谱法、悬浮态高分辨率魔角旋转核磁共振和固态核磁共振光谱法对两种分析物与两种结构相似的手性固定相之间的相互作用进行比较。

Comparisons of the interactions between two analytes and two structurally similar chiral stationary phases using high-performance liquid chromatography, suspended-state high-resolution magic angle spinning nuclear magnetic resonance and solid-state nuclear magnetic resonance spectroscopy.

作者信息

Skogsberg Urban, Händel Heidi, Sanchez Domingo, Albert Klaus

机构信息

Institut für Organische Chemie, Universität Tübingen, Af der Morgenstelle 18, D-72076 Tübingen, Germany.

出版信息

J Chromatogr A. 2004 Jan 16;1023(2):215-23. doi: 10.1016/j.chroma.2003.08.003.

Abstract

A study of the retention behaviour of the enantiomers (R)- and (S)-1,1'-binaphthyl-2,2'-diol as well as (+) and t-)-O,O'-dibenzoyl-tartaric acid was performed using the two chiral stationary phases (CSPs) Kromasil-DMB and Kromasil-TBB. Detailed information about the interactions between the analytes and the two CSPs was obtained from suspended-state HR/MAS transferred NOESY NMR experiments as well as suspended-state HR/MAS 1H NMR titration experiments. Good correlation between the suspended-state HR/MAS NMR experiments and the corresponding HPLC experiments was obtained. This shows that suspended-state HR/MAS NMR as well as solid-state CP/MAS NMR spectroscopy can be used to investigate interactions between stationary phases and analytes under conditions that are similar to those used in HPLC.

摘要

使用两种手性固定相(CSPs)Kromasil-DMB和Kromasil-TBB对(R)-和(S)-1,1'-联萘-2,2'-二醇以及(+)和(-)-O,O'-二苯甲酰基酒石酸对映体的保留行为进行了研究。通过悬浮态HR/MAS转移NOESY NMR实验以及悬浮态HR/MAS 1H NMR滴定实验,获得了有关分析物与两种CSPs之间相互作用的详细信息。悬浮态HR/MAS NMR实验与相应的HPLC实验之间获得了良好的相关性。这表明悬浮态HR/MAS NMR以及固态CP/MAS NMR光谱可用于在与HPLC所用条件相似的条件下研究固定相与分析物之间的相互作用。

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