Overcoming Volume Selectivity of Dipolar Recoupling in Biological Solid-State NMR Spectroscopy

Zdeněk Tošner, Riddhiman Sarkar, Johanna Becker-Baldus, Clemens Glaubitz, Sebastian Wegner, Frank Engelke, Steffen J. Glaser, Bernd Reif

Publikation: Beitrag in FachzeitschriftArtikelBegutachtung

35 Zitate (Scopus)

Abstract

Dipolar recoupling in solid-state NMR is an essential method for establishing correlations between nuclei that are close in space. In applications on protein samples, the traditional experiments like ramped and adiabatic DCP suffer from the fact that dipolar recoupling occurs only within a limited volume of the sample. This selection is dictated by the radiofrequency (rf) field inhomogeneity profile of the excitation solenoidal coil. We employ optimal control strategies to design dipolar recoupling sequences with substantially larger responsive volume and increased sensitivity. We show that it is essential to compensate for additional temporal modulations induced by sample rotation in a spatially inhomogeneous rf field. Such modulations interfere with the pulse sequence and decrease its performance. Using large-scale optimizations we developed pulse schemes for magnetization transfer from amide nitrogen to carbonyl (NCO) as well as aliphatic carbons (NCA). Our experiments yield a signal intensity increased by a factor of 1.5 and 2.0 for NCA and NCO transfers, respectively, compared to conventional ramped DCP sequences. Consistent results were obtained using several biological samples and NMR instruments.

OriginalspracheEnglisch
Seiten (von - bis)14514-14518
Seitenumfang5
FachzeitschriftAngewandte Chemie International Edition in English
Jahrgang57
Ausgabenummer44
DOIs
PublikationsstatusVeröffentlicht - 26 Okt. 2018

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