Characterization of binding affinities in a chromatographic system by suspended state HR/MAS NMR spectroscopy.
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.
Friebolin
Volker
V
University of Tuebingen, Institute of Organic Chemistry, Auf der Morgenstelle 18, 72076 Tuebingen, Germany.
Marten
Silvia
S
Albert
Klaus
K
D001665:Binding Sites; D002851:Chromatography, High Pressure Liquid; D008333:Mandelic Acids / Q000032:analysis / Q000737:chemistry* / Q000302:isolation & purification*; D019906:Nuclear Magnetic Resonance, Biomolecular; D013113:Spin Labels; D013237:Stereoisomerism
D008333:Mandelic Acids; D013113:Spin Labels; C004535:benzylmandelate