Takahashi, H., et al., Optimization of an absolute sensitivity in a glassy matrix during DNP-enhanced multidimensional solid-state NMR experiments. J Magn Reson, 2013. 239C(0): p. 91-99.
Thanks to instrumental and theoretical development, notably the access to high-power and high-frequency microwave sources, high-field dynamic nuclear polarization (DNP) on solid-state NMR currently appears as a promising solution to enhance nuclear magnetization in many different types of systems. In magic-angle-spinning DNP experiments, systems of interest are usually dissolved or suspended in glass-forming matrices doped with polarizing agents and measured at low temperature (down to approximately 100K). In this work, we discuss the influence of sample conditions (radical concentration, sample temperature, etc.) on DNP enhancements and various nuclear relaxation times which affect the absolute sensitivity of DNP spectra, especially in multidimensional experiments. Furthermore, DNP-enhanced solid-state NMR experiments performed at 9.4 T are complemented by high-field CW EPR measurements performed at the same magnetic field. Microwave absorption by the DNP glassy matrix is observed even below the glass transition temperature caused by softening of the glass. Shortening of electron relaxation times due to glass softening and its impact in terms of DNP sensitivity is discussed.
Sensitivity-enhanced solid-state NMR detection of expansin's target in plant cell walls
From The DNP-NMR Blog:
Sensitivity-enhanced solid-state NMR detection of expansin's target in plant cell walls
Wang, T., et al., Sensitivity-enhanced solid-state NMR detection of expansin's target in plant cell walls. Proc Natl Acad Sci U S A, 2013. 110(41): p. 16444-9.
http://www.ncbi.nlm.nih.gov/pubmed/24065828
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11-26-2013 01:19 AM
[NMR paper] Sensitivity-enhanced solid-state NMR detection of expansin's target in plant cell walls.
Sensitivity-enhanced solid-state NMR detection of expansin's target in plant cell walls.
Related Articles Sensitivity-enhanced solid-state NMR detection of expansin's target in plant cell walls.
Proc Natl Acad Sci U S A. 2013 Sep 24;
Authors: Wang T, Park YB, Caporini MA, Rosay M, Zhong L, Cosgrove DJ, Hong M
Abstract
Structure determination of protein binding to noncrystalline macromolecular assemblies such as plant cell walls (CWs) poses a significant structural biology challenge. CWs are loosened during growth by expansin proteins,...
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09-27-2013 03:28 AM
[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
Multidimensional oriented solid-state NMR experiments enable the sequential assignment of uniformly 15N labeled integral membrane proteins in magnetically aligned lipid bilayers
Multidimensional oriented solid-state NMR experiments enable the sequential assignment of uniformly 15N labeled integral membrane proteins in magnetically aligned lipid bilayers
Abstract Oriented solid-state NMR is the most direct methodology to obtain the orientation of membrane proteins with respect to the lipid bilayer. The method consists of measuring 1H-15N dipolar couplings (DC) and 15N anisotropic chemical shifts (CSA) for membrane proteins that are uniformly aligned with respect to the membrane bilayer. A significant advantage of this approach is that tilt and azimuthal...
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10-10-2011 06:27 AM
Signal enhancement for the sensitivity-limited solid state NMR experiments using a continuous, non-uniform acquisition scheme.
Signal enhancement for the sensitivity-limited solid state NMR experiments using a continuous, non-uniform acquisition scheme.
Signal enhancement for the sensitivity-limited solid state NMR experiments using a continuous, non-uniform acquisition scheme.
J Magn Reson. 2011 Aug 30;
Authors: Qiang W
Abstract
We describe a sampling scheme for the two-dimensional (2D) solid state NMR experiments, which can be readily applied to the sensitivity-limited samples. The sampling scheme utilizes continuous, non-uniform sampling profile for the...
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09-21-2011 03:31 PM
[NMR paper] Sensitivity enhancement in two-dimensional solid-state NMR spectroscopy by transverse
Sensitivity enhancement in two-dimensional solid-state NMR spectroscopy by transverse mixing.
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Chemphyschem. 2004 Jun 21;5(6):863-8
Authors: Tycko R
The sensitivity of two-dimensional (2D) 13C-13C solid-state NMR spectroscopy under magic-angle spinning (MAS) is shown to be enhanced by the use of transverse polarization transfer in place of the conventional longitudinal polarization transfer. Experimental results are reported for 2D...
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11-24-2010 09:51 PM
[NMR paper] Resolution enhancement in multidimensional solid-state NMR spectroscopy of proteins u
Resolution enhancement in multidimensional solid-state NMR spectroscopy of proteins using spin-state selection.
Related Articles Resolution enhancement in multidimensional solid-state NMR spectroscopy of proteins using spin-state selection.
J Am Chem Soc. 2003 Oct 1;125(39):11816-7
Authors: Duma L, Hediger S, Brutscher B, Böckmann A, Emsley L
We show that the resolution of homonuclear multidimensional solid-state NMR correlation experiments can be significantly improved using transition selection and spin-state-selective polarization transfer...
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11-24-2010 09:16 PM
[NMR paper] Prospects for resonance assignments in multidimensional solid-state NMR spectra of un
Prospects for resonance assignments in multidimensional solid-state NMR spectra of uniformly labeled proteins.
Related Articles Prospects for resonance assignments in multidimensional solid-state NMR spectra of uniformly labeled proteins.
J Biomol NMR. 1996 Oct;8(3):239-51
Authors: Tycko R
The feasibility of assigning the backbone 15N and 13C NMR chemical shifts in multidimensional magic angle spinning NMR spectra of uniformly isotopically labeled proteins and peptides in unoriented solid samples is assessed by means of numerical simulations....
Optimization of an absolute sensitivity in a glassy matrix during DNP-enhanced multidimensional solid-state NMR experiments
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