Related ArticlesA Novel High-Resolution and Sensitivity-Enhanced Three-Dimensional Solid-State NMR Experiment Under Ultrafast Magic Angle Spinning Conditions.
Sci Rep. 2015;5:11810
Authors: Zhang R, Pandey MK, Nishiyama Y, Ramamoorthy A
Abstract
Although magic angle spinning (MAS) solid-state NMR is a powerful technique to obtain atomic-resolution insights into the structure and dynamics of a variety of chemical and biological solids, poor sensitivity has severely limited its applications. In this study, we demonstrate an approach that suitably combines proton-detection, ultrafast-MAS and multiple frequency dimensions to overcome this limitation. With the utilization of proton-proton dipolar recoupling and double quantum (DQ) coherence excitation/reconversion radio-frequency pulses, very high-resolution proton-based 3D NMR spectra that correlate single-quantum (SQ), DQ and SQ coherences of biological solids have been obtained successfully for the first time. The proposed technique requires a very small amount of sample and does not need multiple radio-frequency (RF) channels. It also reveals information about the proximity between a spin and a certain other dipolar-coupled pair of spins in addition to regular SQ/DQ and SQ/SQ correlations. Although (1)H spectral resolution is still limited for densely proton-coupled systems, the 3D technique is valuable to study dilute proton systems, such as zeolites, small molecules, or deuterated samples. We also believe that this new methodology will aid in the design of a plethora of multidimensional NMR techniques and enable high-throughput investigation of an exciting class of solids at atomic-level resolution.
Closed-cycle cold helium magic-angle spinning for sensitivity-enhanced multi-dimensional solid-state NMR
From The DNP-NMR Blog:
Closed-cycle cold helium magic-angle spinning for sensitivity-enhanced multi-dimensional solid-state NMR
Matsuki, Y., et al., Closed-cycle cold helium magic-angle spinning for sensitivity-enhanced multi-dimensional solid-state NMR. J Magn Reson, 2015. 259: p. 76-81.
http://www.ncbi.nlm.nih.gov/pubmed/26302269
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01-22-2016 04:20 PM
[NMR paper] Restoring Resolution in Biological Solid-State NMR under Conditions of Off-Magic-Angle Spinning.
Restoring Resolution in Biological Solid-State NMR under Conditions of Off-Magic-Angle Spinning.
Related Articles Restoring Resolution in Biological Solid-State NMR under Conditions of Off-Magic-Angle Spinning.
J Phys Chem Lett. 2015 Dec 7;:5040-5044
Authors: Sarkar R, Rodriguez Camargo DC, Pintacuda G, Reif B
Abstract
Spin-state-selective excitation (S3E) experiments allow the selection of individual transitions in a coupled two spin system. We show that in the solid state, the dipole-dipole interaction (DD) between (15)N and...
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12-08-2015 08:28 PM
[NMR paper] Closed-cycle cold helium magic-angle spinning for sensitivity-enhanced multi-dimensional solid-state NMR.
Closed-cycle cold helium magic-angle spinning for sensitivity-enhanced multi-dimensional solid-state NMR.
Related Articles Closed-cycle cold helium magic-angle spinning for sensitivity-enhanced multi-dimensional solid-state NMR.
J Magn Reson. 2015 Aug 12;259:76-81
Authors: Matsuki Y, Nakamura S, Fukui S, Suematsu H, Fujiwara T
Abstract
Magic-angle spinning (MAS) NMR is a powerful tool for studying molecular structure and dynamics, but suffers from its low sensitivity. Here, we developed a novel helium-cooling MAS NMR probe system...
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08-25-2015 08:30 PM
Closed-cycle cold helium magic-angle spinning for sensitivity-enhanced multi-dimensional solid-state NMR
Closed-cycle cold helium magic-angle spinning for sensitivity-enhanced multi-dimensional solid-state NMR
Publication date: Available online 12 August 2015
Source:Journal of Magnetic Resonance</br>
Author(s): Yoh Matsuki, Shinji Nakamura, Shigeo Fukui, Hiroto Suematsu, Toshimichi Fujiwara</br>
Magic-angle spinning (MAS) NMR is a powerful tool for studying molecular structure and dynamics, but suffers from its low sensitivity. Here, we developed a novel helium-cooling MAS NMR probe system adopting a closed-loop gas recirculation mechanism. In addition to...
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08-13-2015 02:00 PM
Recovery of bulk proton magnetization and sensitivity enhancement in ultrafast magic-angle spinning solid-state NMR
From The DNP-NMR Blog:
Recovery of bulk proton magnetization and sensitivity enhancement in ultrafast magic-angle spinning solid-state NMR
A large portion of the magnetization in a CP experiment remains unused after an experiment and different strategies exist to make better use of the proton magnetization. Here the authors show their results of testing 7 different cp schemes. Although not directly related to DNP these techniques are still very valuable to increase the sensitivity of an NMR experiment especially in combination with DNP.
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03-30-2015 06:04 PM
[NMR paper] High-resolution paramagnetically enhanced solid-state NMR spectroscopy of membrane proteins at fast magic angle spinning.
High-resolution paramagnetically enhanced solid-state NMR spectroscopy of membrane proteins at fast magic angle spinning.
Related Articles High-resolution paramagnetically enhanced solid-state NMR spectroscopy of membrane proteins at fast magic angle spinning.
J Biomol NMR. 2013 Dec 13;
Authors: Ward ME, Wang S, Krishnamurthy S, Hutchins H, Fey M, Brown LS, Ladizhansky V
Abstract
Magic angle spinning nuclear magnetic resonance (MAS NMR) is well suited for the study of membrane proteins in membrane mimetic and native membrane...
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12-18-2013 04:00 PM
[NMR paper] Sensitivity and Resolution Enhanced Solid-State NMR for Paramagnetic Systems and Biomolecules under Very Fast Magic Angle Spinning.
Sensitivity and Resolution Enhanced Solid-State NMR for Paramagnetic Systems and Biomolecules under Very Fast Magic Angle Spinning.
Related Articles Sensitivity and Resolution Enhanced Solid-State NMR for Paramagnetic Systems and Biomolecules under Very Fast Magic Angle Spinning.
Acc Chem Res. 2013 Jul 26;
Authors: Parthasarathy S, Nishiyama Y, Ishii Y
Abstract
Recent research in fast magic angle spinning (MAS) methods has drasticallyimproved the resolution and sensitivity of NMR spectroscopy of biomolecules and materials in solids. In...
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07-31-2013 12:00 PM
3D DUMAS: Simultaneous Acquisition of Three-Dimensional Magic Angle Spinning Solid-State NMR Experiments of Proteins
3D DUMAS: Simultaneous Acquisition of Three-Dimensional Magic Angle Spinning Solid-State NMR Experiments of Proteins
Publication year: 2012
Source:Journal of Magnetic Resonance</br>
T. Gopinath, Gianluigi Veglia</br>
Using the DUMAS (Dual acquisition Magic Angle Spinning) solid-state NMR approach, we created new pulse schemes that enable the simultaneous acquisition of three dimensional (3D) experiments on uniformly 13C, 15N labeled proteins. These new experiments exploit the simultaneous cross-polarization (SIM-CP) from 1H to 13C and 15N to acquire two 3D experiments...
A Novel High-Resolution and Sensitivity-Enhanced Three-Dimensional Solid-State NMR Experiment Under Ultrafast Magic Angle Spinning Conditions.
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