Fast magic-angle spinning and partial sample deuteration allows direct detection of 1H in solid-state NMR, yielding significant gains in mass sensitivity. In order to further analyze the spectra, 1H detection requires assignment of the 1H resonances. In this work, resonance assignments of backbone HN and Hα are presented for HET-s(218â??289) fibrils, based on the existing assignment of Cα, Cβ, Câ??, and N resonances. The samples used are partially deuterated for higher spectral resolution, and the shifts in resonance frequencies of Cα and Cβ due to the deuterium isotope effect are investigated. It is shown that the deuterium isotope effect can be estimated and used for assigning resonances of deuterated samples in solid-state NMR, based on known resonances of the protonated protein.
[NMR paper] NMR Spectroscopic Assignment of Backbone and Side-Chain Protons in Fully Protonated Proteins: Microcrystals, Sedimented Assemblies, and Amyloid Fibrils.
NMR Spectroscopic Assignment of Backbone and Side-Chain Protons in Fully Protonated Proteins: Microcrystals, Sedimented Assemblies, and Amyloid Fibrils.
NMR Spectroscopic Assignment of Backbone and Side-Chain Protons in Fully Protonated Proteins: Microcrystals, Sedimented Assemblies, and Amyloid Fibrils.
Angew Chem Int Ed Engl. 2016 Nov 16;:
Authors: Stanek J, Andreas LB, Jaudzems K, Cala D, Lalli D, Bertarello A, Schubeis T, Akopjana I, Kotelovica S, Tars K, Pica A, Leone S, Picone D, Xu ZQ, Dixon NE, Martinez D, Berbon M, El Mammeri N, Noubhani...
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[NMR paper] Further exploration of the conformational space of ?-synuclein fibrils: solid-state NMR assignment of a high-pH polymorph.
Further exploration of the conformational space of ?-synuclein fibrils: solid-state NMR assignment of a high-pH polymorph.
Related Articles Further exploration of the conformational space of ?-synuclein fibrils: solid-state NMR assignment of a high-pH polymorph.
Biomol NMR Assign. 2015 Aug 30;
Authors: Verasdonck J, Bousset L, Gath J, Melki R, Böckmann A, Meier BH
Abstract
Polymorphism is a common and important phenomenon for protein fibrils which has been linked to the appearance of strains in prion and other neurodegenerative...
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09-01-2015 10:48 AM
Simultaneous acquisition of 2D and 3D solid-state NMR experiments for sequential assignment of oriented membrane protein samples
Simultaneous acquisition of 2D and 3D solid-state NMR experiments for sequential assignment of oriented membrane protein samples
Abstract
We present a new method called DAISY (Dual Acquisition orIented ssNMR spectroScopY) for the simultaneous acquisition of 2D and 3D oriented solid-state NMR experiments for membrane proteins reconstituted in mechanically or magnetically aligned lipid bilayers. DAISY utilizes dual acquisition of sine and cosine dipolar or chemical shift coherences and long living 15N longitudinal polarization to obtain two...
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03-08-2015 01:07 AM
[NMR paper] Proton-detected MAS NMR experiments based on dipolar transfers for backbone assignment of highly deuterated proteins.
Proton-detected MAS NMR experiments based on dipolar transfers for backbone assignment of highly deuterated proteins.
Related Articles Proton-detected MAS NMR experiments based on dipolar transfers for backbone assignment of highly deuterated proteins.
J Magn Reson. 2014 Mar 4;242C:180-188
Authors: Chevelkov V, Habenstein B, Loquet A, Giller K, Becker S, Lange A
Abstract
Proton-detected solid-state NMR was applied to a highly deuterated insoluble, non-crystalline biological assembly, the Salmonella typhimurium type iii secretion system...
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03-29-2014 01:00 PM
Proton-detected MAS NMR experiments based on dipolar transfers for backbone assignment of highly deuterated proteins
Proton-detected MAS NMR experiments based on dipolar transfers for backbone assignment of highly deuterated proteins
Publication date: Available online 4 March 2014
Source:Journal of Magnetic Resonance</br>
Author(s): Veniamin Chevelkov , Birgit Habenstein , Antoine Loquet , Karin Giller , Stefan Becker , Adam Lange</br>
Proton-detected solid-state NMR was applied to a highly deuterated insoluble, non-crystalline biological assembly, the Salmonella typhimurium type iii secretion system (T3SS) needle. Spectra of very high resolution and sensitivity were obtained...
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Deuterium isotope shifts for backbone 1H, 15N and 13C nuclei in intrinsically disordered protein α-synuclein
Deuterium isotope shifts for backbone 1H, 15N and 13C nuclei in intrinsically disordered protein α-synuclein
Abstract Intrinsically disordered proteins (IDPs) are abundant in nature and characterization of their potential structural propensities remains a widely pursued but challenging task. Analysis of NMR secondary chemical shifts plays an important role in such studies, but the output of such analyses depends on the accuracy of reference random coil chemical shifts. Although uniform perdeuteration of IDPs can dramatically increase spectral resolution, a feature particularly...
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[NMR paper] Expression of deuterium-isotope-labelled protein in the yeast pichia pastoris for NMR
Expression of deuterium-isotope-labelled protein in the yeast pichia pastoris for NMR studies.
Related Articles Expression of deuterium-isotope-labelled protein in the yeast pichia pastoris for NMR studies.
J Biomol NMR. 2000 Aug;17(4):337-47
Authors: Morgan WD, Kragt A, Feeney J
Deuterium isotope labelling is important for NMR studies of large proteins and complexes. Many eukaryotic proteins are difficult to express in bacteria, but can be efficiently produced in the methylotrophic yeast Pichia pastoris. In order to facilitate NMR studies of...
Partially-deuterated samples of HET-s(218â??289) fibrils: assignment and deuterium isotope effect
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