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Characterization of binding affinities in a chromatographic system by suspended state HR/MAS NMR spectroscopy

2009; Wiley; Volume: 48; Issue: 2 Linguagem: Inglês

10.1002/mrc.2551

1097-458X

Volker Friebolin, Silvia Marten, Klaus Albert,

Microfluidic and Capillary Electrophoresis Applications

Abstract 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. Copyright © 2009 John Wiley & Sons, Ltd.