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 yielding a high resolution spectrum. This has a range of applications as exemplified for different systems such as large proteins, intrinsically disordered polypeptides and proteins with a paramagnetic centre.
Content Type Journal Article
Category Article
Pages 1-10
DOI 10.1007/s10858-012-9647-0
Authors
Garima Jaipuria, NMR Research Centre, Indian Institute of Science, Bangalore, 560012 India
Nitin Prakash Lobo, NMR Research Centre, Indian Institute of Science, Bangalore, 560012 India
Divya Shet, NMR Research Centre, Indian Institute of Science, Bangalore, 560012 India
Hanudatta S. Atreya, NMR Research Centre, Indian Institute of Science, Bangalore, 560012 India
Selective editing of Val and Leu methyl groups in high molecular weight protein NMR
Selective editing of Val and Leu methyl groups in high molecular weight protein NMR
Abstract The development of methyl-TROSY approaches and specific 13Câ??1H labeling of Ile, Leu and Val methyl groups in highly deuterated proteins has made it possible to study high molecular weight proteins, either alone or in complexes, using solution nuclear magnetic resonance (NMR) spectroscopy. Here we present 2-dimensional (2D) and 3-dimensional (3D) NMR experiments designed to achieve complete separation of the methyl resonances of Val and Leu, labeled using the same precursor, α-ketoisovalerate...
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05-01-2012 07:06 AM
Ultra-high resolution in MAS solid-state NMR of perdeuterated proteins: Implications for structure and dynamics
Ultra-high resolution in MAS solid-state NMR of perdeuterated proteins: Implications for structure and dynamics
Publication year: 2012
Source:Journal of Magnetic Resonance, Volume 216</br>
Bernd Reif</br>
High resolution proton spectra are obtained in MAS solid-state NMR in case samples are prepared using perdeuterated protein and D2O in the recrystallization buffer. Deuteration reduces drastically 1H, 1H dipolar interactions and allows to obtain amide proton line widths on the order of 20 Hz. Similarly, high-resolution proton spectra of aliphatic groups can be obtained...
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03-13-2012 03:33 PM
Efficient Acquisition of High-Resolution 4-D Diagonal-Suppressed Methyl-Methyl NOESY for Large Proteins
Efficient Acquisition of High-Resolution 4-D Diagonal-Suppressed Methyl-Methyl NOESY for Large Proteins
Publication year: 2012
Source:Journal of Magnetic Resonance</br>
Jie Wen, Jihui Wu, Pei Zhou</br>
The methyl-methyl NOESYexperimentplays an important role in determiningthe global folds of large proteins. Despite the high sensitivity of this experiment, the analysisof methyl-methyl NOEs is frequently hindered by the limited chemical shift dispersion of methyl groups, particularly methyl protons. Thismakes it difficult to unambiguously assign all of the methyl-methyl...
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03-10-2012 10:54 AM
Ultra-high resolution in MAS solid-state NMR of perdeuterated proteins: Implications for Structure and Dynamics
Ultra-high resolution in MAS solid-state NMR of perdeuterated proteins: Implications for Structure and Dynamics
Publication year: 2012
Source: Journal of Magnetic Resonance, Available online 5 January 2012</br>
Bernd*Reif</br>
http://www.sciencedirect.com/cache/MiamiImageURL/1-s2.0-S1090780711005969-fx1.sml</br></br></br>
Source: Journal of Magnetic Resonance
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01-07-2012 03:12 PM
Three-dimensional deuterium-carbon correlation experiments for high-resolution solid-state MAS NMR spectroscopy of large proteins
Three-dimensional deuterium-carbon correlation experiments for high-resolution solid-state MAS NMR spectroscopy of large proteins
Abstract Well-resolved 2Hâ??13C correlation spectra, reminiscent of 1Hâ??13C correlations, are obtained for perdeuterated ubiquitin and for perdeuterated outer-membrane protein G (OmpG) from E. coli by exploiting the favorable lifetime of 2H double-quantum (DQ) states. Sufficient signal-to-noise was achieved due to the short deuterium T 1, allowing for high repetition rates and enabling 3D experiments with a 2Hâ??13C transfer step in a reasonable time....
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11-01-2011 01:52 AM
An optimized isotopic labelling strategy of isoleucine-?(2) methyl groups for solution NMR studies of high molecular weight proteins.
An optimized isotopic labelling strategy of isoleucine-?(2) methyl groups for solution NMR studies of high molecular weight proteins.
An optimized isotopic labelling strategy of isoleucine-?(2) methyl groups for solution NMR studies of high molecular weight proteins.
Chem Commun (Camb). 2011 Jul 26;
Authors: Ayala I, Hamelin O, Amero C, Pessey O, Plevin MJ, Gans P, Boisbouvier J
An efficient synthetic route is proposed to produce 2-hydroxy-2-ethyl-3-oxobutanoate for the specific labelling of Ile methyl-?(2) groups in proteins. The (2)H,...
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07-28-2011 10:51 AM
[NMR paper] Towards high-resolution solid-state NMR on large uniformly 15N- and [13C,15N]-labeled
Towards high-resolution solid-state NMR on large uniformly 15N- and -labeled membrane proteins in oriented lipid bilayers.
Related Articles Towards high-resolution solid-state NMR on large uniformly 15N- and -labeled membrane proteins in oriented lipid bilayers.
J Biomol NMR. 2002 Mar;22(3):225-47
Authors: Vosegaard T, Nielsen NC
Based on exact numerical simulations, taking into account isotropic and conformation-dependent anisotropic nuclear spin interactions, we systematically analyse the prospects for high-resolution solid-state NMR on...
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11-24-2010 08:49 PM
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...
High resolution methyl selective 13C-NMR of proteins in solution and solid state
Linear Mode
