Publication date: Available online 13 September 2013 Source:Journal of Magnetic Resonance
Author(s): Jochem O. Struppe , Chen Yang , Yachong Wang , Roy V. Hernandez , Lisa M. Shamansky , Leonard J. Mueller
Sensitivity and resolution are the two fundamental obstacles to extending solid-state nuclear magnetic resonance to even larger protein systems. Here, a novel long-observation-window band-selective homonuclear decoupling (LOW BASHD) scheme is introduced that increases resolution up to a factor of 3 and sensitivity up to 1.8 by decoupling backbone alpha-carbon (C?) and carbonyl (C’) nuclei in U-13C-labeled proteins during direct 13C acquisition. This approach introduces short (<200 ?s) pulse breaks into much longer (~8 ms) sampling windows to efficiently refocus the J-coupling interaction during detection while avoiding the deleterious effects on sensitivity inherent in rapid stroboscopic band-selective homonuclear decoupling techniques. A significant advantage of LOW BASHD detection is that it can be directly incorporated into existing correlation methods, as illustrated here for 2D CACO, NCO, and NCA correlation spectroscopy applied to the ?1 immunoglobulin binding domain of protein G and 3D CBCACO correlation spectroscopy applied to the ?-subunit of tryptophan synthase. Graphical abstract
Sensitivity and Resolution Enhancement of Oriented Solid-State NMR: Application to Membrane Proteins
Sensitivity and Resolution Enhancement of Oriented Solid-State NMR: Application to Membrane Proteins
Publication date: Available online 12 August 2013
Source:Progress in Nuclear Magnetic Resonance Spectroscopy</br>
Author(s): T. Gopinath , Kaustubh R. Mote , Gianluigi Veglia</br>
Oriented solid-state NMR (O-ssNMR) spectroscopy is a major technique for the high-resolution analysis of the structure and topology of transmembrane proteins in native-like environments. Unlike magic angle spinning (MAS) techniques, O-ssNMR spectroscopy requires membrane protein...
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[NMR paper] Refocused continuous-wave decoupling: a new approach to heteronuclear dipolar decoupling in solid-state NMR spectroscopy.
Refocused continuous-wave decoupling: a new approach to heteronuclear dipolar decoupling in solid-state NMR spectroscopy.
http://www.bionmr.com//www.ncbi.nlm.nih.gov/corehtml/query/egifs/http:--link.aip.org-jhtml-linkto.gif Related Articles Refocused continuous-wave decoupling: a new approach to heteronuclear dipolar decoupling in solid-state NMR spectroscopy.
J Chem Phys. 2012 Dec 7;137(21):214202
Authors: Vinther JM, Nielsen AB, Bjerring M, van Eck ER, Kentgens AP, Khaneja N, Nielsen NC
Abstract
A novel strategy for heteronuclear dipolar...
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06-01-2013 02:03 PM
[NMR paper] Efficient CO-CA transfer in highly deuterated proteins by band-selective homonuclear cross-polarization
Efficient CO-CA transfer in highly deuterated proteins by band-selective homonuclear cross-polarization
Available online 14 March 2013
Publication year: 2013
Source:Journal of Magnetic Resonance</br>
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Robust and efficient band-selective magnetization transfer between CO and CA spins can be achieved in highly deuterated solid proteins by dipolar-based homonuclear cross polarization. The approach is designed for moderate magic-angle spinning rates and high external magnetic fields where the isotropic chemical shift difference of CO and CA considerably exceeds the...
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03-16-2013 02:22 AM
Recombinant proteins incorporating short non-native extensions may display increased aggregation propensity as detected by high resolution NMR spectroscopy
Recombinant proteins incorporating short non-native extensions may display increased aggregation propensity as detected by high resolution NMR spectroscopy
26 October 2012
Publication year: 2012
Source:Biochemical and Biophysical Research Communications, Volume 427, Issue 3</br>
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The use of a recombinant protein to investigate the function of the native molecule requires that the former be obtained with the same amino acid sequence as the template. However, in many cases few additional residues are artificially introduced for cloning or purification purposes,...
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02-03-2013 10:13 AM
High resolution methyl selective 13C-NMR of proteins in solution and solid state
High resolution methyl selective 13C-NMR of proteins in solution and solid state
Abstract New 13C-detected NMR experiments have been devised for molecules in solution and solid state, which provide chemical shift correlations of methyl groups with high resolution, selectivity and sensitivity. The experiments achieve selective methyl detection by exploiting the one bond J-coupling between the 13C-methyl nucleus and its directly attached 13C spin in a molecule. In proteins such correlations edit the 13C-resonances of different methyl containing residues into distinct spectral regions...
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07-13-2012 10:46 PM
Straightforward, effective calibration of SPINAL-64 decoupling results in the enhancement of sensitivity and resolution of biomolecular solid-state NMR.
Straightforward, effective calibration of SPINAL-64 decoupling results in the enhancement of sensitivity and resolution of biomolecular solid-state NMR.
Straightforward, effective calibration of SPINAL-64 decoupling results in the enhancement of sensitivity and resolution of biomolecular solid-state NMR.
J Magn Reson. 2010 Dec 31;
Authors: Comellas G, Lopez JJ, Nieuwkoop AJ, Lemkau LR, Rienstra CM
We describe a simple yet highly effective optimization strategy for SPINAL-64 (1)H decoupling conditions for magic-angle spinning solid-state NMR. With...
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02-08-2011 06:28 PM
Straightforward, effective calibration of SPINAL-64 decoupling results in the enhancement of sensitivity and resolution of biomolecular solid-state NMR
Straightforward, effective calibration of SPINAL-64 decoupling results in the enhancement of sensitivity and resolution of biomolecular solid-state NMR
Publication year: 2010
Source: Journal of Magnetic Resonance, In Press, Accepted Manuscript, Available online 31 December 2010</br>
Gemma, Comellas , Jakob J., Lopez , Andrew J., Nieuwkoop , Luisel R., Lemkau , Chad M., Rienstra</br>
We describe a simple yet highly effective optimization strategy for SPINAL-64 1H decoupling conditions for magic-angle spinning solid-state NMR. With adjustment of the phase angles in a coupled manner,...
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01-01-2011 08:57 AM
High Resolution 1H Detected 1H,13C Correlation Spectra in MAS Solid-State NMR using Deuterated Proteins with Selective 1H,2H Isotopic Labeling of Methyl Groups
High Resolution <SUP>1</SUP>H Detected <SUP>1</SUP>H,<SUP>13</SUP>C Correlation Spectra in MAS Solid-State NMR using Deuterated Proteins with Selective <SUP>1</SUP>H,<SUP>2</SUP>H Isotopic Labeling of Methyl Groups
Vipin Agarwal, Anne Diehl, Nikolai Skrynnikov, and Bernd Reif
J. Am. Chem. Soc.; 2006; 128(39) pp 12620 - 12621;
Abstract:
MAS solid-state NMR experiments applied to biological solids are still hampered by low sensitivity and resolution. In this work, we employ a deuteration scheme in which individual methyl groups are selectively protonated. This labeling scheme...
Long-Observation-Window Band-Selective Homonuclear Decoupling: Increased Sensitivity and Resolution in Solid-State NMR Spectroscopy of Proteins
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