Skogsberg Urban, Händel Heidi, Sanchez Domingo, Albert Klaus
Institut für Organische Chemie, Universität Tübingen, Af der Morgenstelle 18, D-72076 Tübingen, Germany.
J Chromatogr A. 2004 Jan 16;1023(2):215-23. doi: 10.1016/j.chroma.2003.08.003.
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.
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。