Rapid Structural Analysis of Minute Quantities of Organic Solids by Exhausting 1H Polarization in Solid-State NMR Spectroscopy Under Fast Magic Angle Spinning

作者：Yan, Zhiwei; Zhang, Rongchun^*

来源：Journal of Physical Chemistry Letters, 2021, 12(50): 12067-12074.

DOI：10.1021/acs.jpclett.1c03672

• CROSS-POLARIZATION
• SIMULTANEOUS ACQUISITION
• FLIP-BACK
• SENSITIVITY
• RESOLUTION
• RESONANCE
• ENHANCEMENT
• PROTEINS
• SPECTRA
• PHASE

Solid-state nuclear magnetic resonance (NMR) often suffers from significant limitations due to the inherent low signal sensitivity when low-gamma nuclei are involved. Herein, we report an elegant solid-state NMR approach for rapid structural analysis of minute amounts of organic solids. By encoding staggered chemical shift evolution in the indirect dimension and staggered acquisition in the 'H dimension, a proton-detected homonuclear H-1/H-1 and heteronuclear C-13/H-1 chemical shift correlation (HETCOR) spectrum can be obtained simultaneously in a single experiment at a fast magic-angle-spinning (MAS) condition with barely increasing the experimental time. We further show that during the conventional 'H-detected HETCOR experimental time, multiple homonuclear H-1/H-1 correlation spectra can be recorded in addition to the HETCOR spectrum, enabling the determination of H-1-H-1 distances. We establish that abundant H-1 polarization can be efficiently manipulated and fully utilized in proton-detected solid-state NMR spectroscopy for extraction of more critical structural information and thus reduction of the total experimental time.