Probe design for high sensitivity proton-detected solid-state NMR

Abstract

Proton (¹H) detection methodologies in solid-state NMR (SSNMR) have revolutionized the field allowing for probing of new frontiers in determining the structure and dynamics within biological systems and materials. While approaches that maximally leverage the high gyromagnetic ratio of ¹H detection have enhanced sensitivity and resolution of SSNMR experiments, the radiofrequency (rf) circuit of magic-angle spinning (MAS) probes is not well optimized for ¹H detection, limiting the overall signal-to-noise ratio (SNR). Rather, SSNMR probes have historically been optimized for lower gamma nuclei such as ¹³C and below. Here we present a design with an inner coil for proton (¹H) to maximize ¹H sensitivity. Optimizing the ¹H channel resulted in a 1.33–2-fold increase in SNR with ¹H detection in a one-dimensional experiment. An outer coil is tuned to the ¹³C and ¹⁵N frequencies, with excellent B₁ homogeneity on all three channels. Using this design, we find that the sensitivity scales better than the theoretical expectations from 600 MHz to 750 MHz, due to a combination of the improved rf efficiency and B₁ homogeneity. We also demonstrate these improvements on a model protein system (GB1) with a 4D experiment collected in less than a day.