DNP-enhanced solid-state NMR has been shown to hold great potential for functional studies of membrane proteins at low temperatures due to its great sensitivity improvement. There are however numerous applications, for which experiments at ambient temperature are desirable and which would also benefit from DNP signal enhancement. Here, we demonstrate as a proof of concept that a significant signal increase for lipid bilayers under room temperature conditions can be achieved by utilizing the Overhauser effect. Experiments were carried out on aligned bilayers at 400 MHz/263 GHz using a stripline structure combined with a Fabry-Perot microwave resonator. A signal enhancement of protons of up to -10 was observed. Our results demonstrate that Overhauser DNP at high field pro-vides efficient polarization transfer within insoluble samples, which is driven by fast local molecular fluc-tuations. Furthermore, our experimental setup offers an attractive option for DNP-enhanced solid-state NMR on ordered membranes and provides a general perspective towards DNP at ambient temperatures.
DynamicNuclear Polarization-Enhanced NMR on AlignedLipid Bilayers at Ambient Temperature
DynamicNuclear Polarization-Enhanced NMR on AlignedLipid Bilayers at Ambient Temperature
Orawan Jakdetchai, Vasyl Denysenkov, Johanna Becker-Baldus, Bercem Dutagaci, Thomas F. Prisner and Clemens Glaubitz
http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jacsat/0/jacsat.ahead-of-print/ja509799s/20141023/images/medium/ja-2014-09799s_0003.gif
Journal of the American Chemical Society
DOI: 10.1021/ja509799s
http://feeds.feedburner.com/~ff/acs/jacsat?d=yIl2AUoC8zA
http://feeds.feedburner.com/~r/acs/jacsat/~4/S2bKDta85YQ
nmrlearner
Journal club
0
10-24-2014 07:18 PM
[NMR paper] DNP-enhanced NMR on aligned Lipid Bilayers at ambient Temperature.
DNP-enhanced NMR on aligned Lipid Bilayers at ambient Temperature.
Related Articles DNP-enhanced NMR on aligned Lipid Bilayers at ambient Temperature.
J Am Chem Soc. 2014 Oct 21;
Authors: Jakdetchai O, Denysenkov V, Becker-Baldus J, Dutagaci B, Prisner T, Glaubitz C
Abstract
DNP-enhanced solid-state NMR has been shown to hold great potential for functional studies of membrane proteins at low temperatures due to its great sensitivity improvement. There are however numerous applications, for which experiments at ambient temperature...
nmrlearner
Journal club
0
10-22-2014 12:34 PM
[NMR paper] Dipolar Assisted Assignment Protocol (DAAP) for MAS solid-state NMR of rotationally aligned membrane proteins in phospholipid bilayers.
Dipolar Assisted Assignment Protocol (DAAP) for MAS solid-state NMR of rotationally aligned membrane proteins in phospholipid bilayers.
Dipolar Assisted Assignment Protocol (DAAP) for MAS solid-state NMR of rotationally aligned membrane proteins in phospholipid bilayers.
J Magn Reson. 2014 Mar 1;242C:224-232
Authors: Das BB, Zhang H, Opella SJ
Abstract
A method for making resonance assignments in magic angle spinning solid-state NMR spectra of membrane proteins that utilizes the range of heteronuclear dipolar coupling...
nmrlearner
Journal club
0
04-06-2014 02:01 AM
Dipolar Assisted Assignment Protocol (DAAP) for MAS solid-state NMR of Rotationally Aligned Membrane Proteins in Phospholipid Bilayers
Dipolar Assisted Assignment Protocol (DAAP) for MAS solid-state NMR of Rotationally Aligned Membrane Proteins in Phospholipid Bilayers
Publication date: Available online 1 March 2014
Source:Journal of Magnetic Resonance</br>
Author(s): Bibhuti B. Das , Hua Zhang , Stanley J. Opella</br>
A method for making resonance assignments in magic angle spinning solid-state NMR spectra of membrane proteins that utilizes the range of hetero-nuclear dipolar coupling frequencies in combination with conventional chemical shift based assignment methods is demonstrated. The...
nmrlearner
Journal club
0
03-01-2014 11:11 AM
Proton polarization in photo-excited aromatic molecule at room temperature enhanced by intense optical source and temperature control
From The DNP-NMR Blog:
Proton polarization in photo-excited aromatic molecule at room temperature enhanced by intense optical source and temperature control
Sakaguchi, S., et al., Proton polarization in photo-excited aromatic molecule at room temperature enhanced by intense optical source and temperature control. Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms, 2013. 317(0): p. 679-684.
http://www.sciencedirect.com/science/article/pii/S0168583X13008872
nmrlearner
News from NMR blogs
0
01-23-2014 01:37 AM
Proton polarization in photo-excited aromatic molecule at room temperature enhanced by intense optical source and temperature control
From The DNP-NMR Blog:
Proton polarization in photo-excited aromatic molecule at room temperature enhanced by intense optical source and temperature control
Sakaguchi, S., et al., Proton polarization in photo-excited aromatic molecule at room temperature enhanced by intense optical source and temperature control. Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms, 2013(0).
http://www.sciencedirect.com/science/article/pii/S0168583X13008872
nmrlearner
News from NMR blogs
0
11-21-2013 01:14 AM
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...
nmrlearner
Journal club
0
10-10-2011 06:27 AM
Molecular Dynamics of Proteorhodopsin in Lipid Bilayers by Solid-State NMR.
Molecular Dynamics of Proteorhodopsin in Lipid Bilayers by Solid-State NMR.
Molecular Dynamics of Proteorhodopsin in Lipid Bilayers by Solid-State NMR.
J Am Chem Soc. 2011 Mar 14;
Authors: Yang J, Aslimovska L, Glaubitz C
Environmental factors such as temperature, hydration, and lipid bilayer properties are tightly coupled to the dynamics of membrane proteins. So far, site-resolved data visualizing the protein's response to alterations in these factors are rare, and conclusions had to be drawn from dynamic data averaged over the whole protein...