25-30 August 2019
Henry Ford Building
Europe/Berlin timezone

Strategies for $^{1}$H-detected dynamic nuclear polarization magic-angle spinning NMR.

Not scheduled
Harnack House and Henry Ford Building

Harnack House and Henry Ford Building

Board: 77
Poster Posters


Dr Maria Concistre (University of Southampton)


Over the last two decades there have been remarkable advances in solid-state NMR (SSNMR) experiments for the characterization of protein structure and function. However still at this time, some applications of SSNMR are complicated, impaired or made impossible by the intrinsic low sensitivity of the technique. Moreover, most protein studies in solid-state NMR have so far relied on labelling and detection of nuclei with low gyromagnetic ratios including $^{13}$C and $^{15}$N, a technique which is time consuming, costly and not always feasible.
To overcome these limitations, advances are being made in two, potentially complementary, areas: dynamic nuclear polarization (DNP) and proton-detect fast-MAS NMR. Extending these approaches to large systems, complex biomaterials and unlabeled samples require a combination of these two methodologies. This is the ultimate aim of this work but such combination is not as trivial as it may sound. On the one hand, proton detection in solids is notably difficult since the density of proton within biomaterials results in a strong network of homonuclear dipolar couplings which significantly compromise resolution. On the other hand, MAS-DNP is typically run at 100K mostly using radicals exploiting the cross-effect and despite improvements in technology, the spinning speeds available on DNP systems still lag behind those of conventional fast-MAS probes for $^{1}$H detection. On a positive note, the development of new radicals for use at high magnetic fields and under fast-MAS is an area of active research.
In this contribution we address some of these challenges and the advances done towards $^{1}$H-detected DNP-enhanced MAS. Working on a model sample made by the protein GB3 expressed in different labelled varieties and degree of deuteration, we demonstrate that proton-detected MAS-DNP may be used to study biomaterials in ‘widely’ available commercial instruments.

Primary authors

Dr Maria Concistre (University of Southampton) Dr Subhradip Paul (University of Nottingham) Dr Philip Williamson (University of Southampton)

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