We present a new solid-state NMR proton-detected three-dimensional experiment dedicated to the observation of protein proton side chain resonances in nano-liter volumes. The experiment takes advantage of very fast magic angle spinning and double quantum 13Câ??13C transfer to establish efficient (H)CCH correlations detected on side chain protons. Our approach is demonstrated on the HET-s prion domain in its functional amyloid fibrillar form, fully protonated, with a sample amount of less than 500 µg using a MAS frequency of 70Â*kHz. The majority of aliphatic and aromatic side chain protons (70%) are observable, in addition to Hα resonances, in a single experiment providing a complementary approach to the established proton-detected amide-based multidimensional solid-state NMR experiments for the study and resonance assignment of biosolid samples, in particular for aromatic side chain resonances.
[NMR paper] Selective (1)H-(1)H Distance Restraints in Fully Protonated Proteins by Very Fast Magic-Angle Spinning Solid-State NMR.
Selective (1)H-(1)H Distance Restraints in Fully Protonated Proteins by Very Fast Magic-Angle Spinning Solid-State NMR.
Related Articles Selective (1)H-(1)H Distance Restraints in Fully Protonated Proteins by Very Fast Magic-Angle Spinning Solid-State NMR.
J Phys Chem Lett. 2017 May 11;:
Authors: Jain MG, Lalli D, Stanek J, GOwda CM, Prakash S, Schwarzer TS, Schubeis T, Castiglione K, Andreas LB, Madhu PK, Pintacuda G, Agarwal V
Abstract
Very fast magic-angle spinning (MAS>80 kHz) NMR spectroscopy combined with high field magnets...
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05-12-2017 05:13 PM
[NMR paper] Backbone assignment of perdeuterated proteins by solid-state NMR using proton detection and ultrafast magic-angle spinning.
Backbone assignment of perdeuterated proteins by solid-state NMR using proton detection and ultrafast magic-angle spinning.
Related Articles Backbone assignment of perdeuterated proteins by solid-state NMR using proton detection and ultrafast magic-angle spinning.
Nat Protoc. 2017 Apr;12(4):764-782
Authors: Fricke P, Chevelkov V, Zinke M, Giller K, Becker S, Lange A
Abstract
Solid-state NMR (ssNMR) is a technique that allows the study of protein structure and dynamics at atomic detail. In contrast to X-ray crystallography and...
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03-10-2017 04:23 PM
[NMR paper] Structure of fully protonated proteins by proton-detected magic-angle spinning NMR.
Structure of fully protonated proteins by proton-detected magic-angle spinning NMR.
Related Articles Structure of fully protonated proteins by proton-detected magic-angle spinning NMR.
Proc Natl Acad Sci U S A. 2016 Aug 3;
Authors: Andreas LB, Jaudzems K, Stanek J, Lalli D, Bertarello A, Le Marchand T, Cala-De Paepe D, Kotelovica S, Akopjana I, Knott B, Wegner S, Engelke F, Lesage A, Emsley L, Tars K, Herrmann T, Pintacuda G
Abstract
Protein structure determination by proton-detected magic-angle spinning (MAS) NMR has focused on...
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08-05-2016 12:26 PM
[NMR paper] Proton-detected solid-state NMR spectroscopy of fully protonated proteins at slow to moderate magic-angle spinning frequencies.
Proton-detected solid-state NMR spectroscopy of fully protonated proteins at slow to moderate magic-angle spinning frequencies.
Related Articles Proton-detected solid-state NMR spectroscopy of fully protonated proteins at slow to moderate magic-angle spinning frequencies.
J Magn Reson. 2015 Nov 9;261:149-156
Authors: Mote KR, Madhu PK
Abstract
(1)H-detection offers a substitute to the sensitivity-starved experiments often used to characterize biomolecular samples using magic-angle spinning solid-state NMR spectroscopy...
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11-19-2015 05:22 PM
Proton-detected solid-state NMR spectroscopy of fully protonated proteins at slow to moderate magic-angle spinning frequencies
Proton-detected solid-state NMR spectroscopy of fully protonated proteins at slow to moderate magic-angle spinning frequencies
Publication date: Available online 9 November 2015
Source:Journal of Magnetic Resonance</br>
Author(s): Kaustubh R. Mote, Perunthiruthy K. Madhu</br>
1 H-detection offers a substitute to the sensitivity-starved experiments often used to characterize biomolecular samples using magic-angle spinning solid-state NMR spectroscopy (MAS-ssNMR). To mitigate the effects of the strong 1 H- 1 H dipolar coupled network that...
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11-10-2015 09:10 AM
[NMR paper] Nano-Mole Scale Side-Chain Signal Assignment by 1H-Detected Protein Solid-State NMR by Ultra-Fast Magic-Angle Spinning and Stereo-Array Isotope Labeling.
Nano-Mole Scale Side-Chain Signal Assignment by 1H-Detected Protein Solid-State NMR by Ultra-Fast Magic-Angle Spinning and Stereo-Array Isotope Labeling.
http://www.bionmr.com//www.ncbi.nlm.nih.gov/corehtml/query/egifs/http:--www.plosone.org-images-pone_120x30.png Related Articles Nano-Mole Scale Side-Chain Signal Assignment by 1H-Detected Protein Solid-State NMR by Ultra-Fast Magic-Angle Spinning and Stereo-Array Isotope Labeling.
PLoS One. 2015;10(4):e0122714
Authors: Wang S, Parthasarathy S, Nishiyama Y, Endo Y, Nemoto T, Yamauchi K, Asakura T,...
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04-11-2015 12:04 AM
Fast magic angle spinning NMR with heteronucleus detection for resonance assignments and structural characterization of fully protonated proteins
Fast magic angle spinning NMR with heteronucleus detection for resonance assignments and structural characterization of fully protonated proteins
Abstract
Heteronucleus-detected dipolar based correlation spectroscopy is established for assignments of 1H, 13C, and 15N resonances and structural analysis in fully protonated proteins. We demonstrate that 13C detected 3D experiments are highly efficient and permit assignments of the majority of backbone resonances, as shown in an 89-residue dynein light chain 8, LC8 protein. With these experiments, we...
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11-11-2014 11:57 AM
[NMR paper] Fast magic angle spinning NMR with heteronucleus detection for resonance assignments and structural characterization of fully protonated proteins.
Fast magic angle spinning NMR with heteronucleus detection for resonance assignments and structural characterization of fully protonated proteins.
Related Articles Fast magic angle spinning NMR with heteronucleus detection for resonance assignments and structural characterization of fully protonated proteins.
J Biomol NMR. 2014 Nov 9;
Authors: Guo C, Hou G, Lu X, O'Hare B, Struppe J, Polenova T
Abstract
Heteronucleus-detected dipolar based correlation spectroscopy is established for assignments of (1)H, (13)C, and (15)N...
Detection of side-chain proton resonances of fully protonated biosolids in nano-litre volumes by magic angle spinning solid-state NMR
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