We introduce an analytical method that combines in one pot the advantages of column chromatography separation and NMR structural analysis. The separation of the NMR spectra of the components of a mixture can be achieved according to their apparent diffusion rates [James, T. L. and McDonald, G. G. (1973) J. Magn. Reson. 58, 5861]. We show that the separation of the spectral components, corresponding to single molecular species, can be enhanced by order of magnitudes upon addition of a typical stationary phase used in HPLC. The solid phase imbibed by the mixture for analysis is an heterogeneous ensemble, so that solidstate NMR methods (high-resolution magic angle spinning) are necessary to recover high-resolution spectra. We demonstrate applications of this combination of high-resolution magic angle spinning and NMR diffusometry on test mixtures for direct (silica gel) and inverse (C18) columns. However, many common chromatographic supports available for HPLC should be readily adaptable for use with this technique
Enhanced diffusion-edited NMR spectroscopy of mixtures using chromatographic stationary phases
2003
Abstract
We introduce an analytical method that combines in one pot the advantages of column chromatography separation and NMR structural analysis. The separation of the NMR spectra of the components of a mixture can be achieved according to their apparent diffusion rates [James, T. L. and McDonald, G. G. (1973) J. Magn. Reson. 58, 5861]. We show that the separation of the spectral components, corresponding to single molecular species, can be enhanced by order of magnitudes upon addition of a typical stationary phase used in HPLC. The solid phase imbibed by the mixture for analysis is an heterogeneous ensemble, so that solidstate NMR methods (high-resolution magic angle spinning) are necessary to recover high-resolution spectra. We demonstrate applications of this combination of high-resolution magic angle spinning and NMR diffusometry on test mixtures for direct (silica gel) and inverse (C18) columns. However, many common chromatographic supports available for HPLC should be readily adaptable for use with this techniqueI documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
