In recent years, Dynamic Nuclear Polarization (DNP) has re-emerged as a means to ameliorate the inherent problem of low sensitivity in nuclear magnetic resonance (NMR). Here, we present a novel approach to DNP enhanced liquid-state NMR based on rapid melting of a solid hyperpolarized sample followed by 'in situ' NMR detection. This method is applicable to small (10nl to 1mul) sized samples in a microfluidic setup. The method combines generic DNP enhancement in the solid state with the high sensitivity of stripline (1)H NMR detection in the liquid state. Fast cycling facilitates options for signal averaging or 2D structural analysis. Preliminary tests show solid-state (1)H enhancement factors of up to 500 for H2O/D2O/d6-glycerol samples doped with TEMPOL radicals. Fast paramagnetic relaxation with nitroxide radicals, In nonpolar solvents such as toluene, we find proton enhancement factors up to 400 with negligible relaxation losses in the liquid state, using commercially available BDPA radicals. A total recycling delay (including sample freezing, DNP polarization and melting) of about 5s can be used. The present setup allows for a fast determination of the hyper-polarization as function of the microwave frequency and power. Even at the relatively low field of 3.4T, the method of rapid melting DNP can facilitate the detection of small quantities of molecules in the picomole regime.
PRESTO polarization transfer to quadrupolar nuclei: implications for dynamic nuclear polarization
From The DNP-NMR Blog:
PRESTO polarization transfer to quadrupolar nuclei: implications for dynamic nuclear polarization
Perras, F.A., T. Kobayashi, and M. Pruski, PRESTO polarization transfer to quadrupolar nuclei: implications for dynamic nuclear polarization. Phys Chem Chem Phys, 2015. 17(35): p. 22616-22.
http://www.ncbi.nlm.nih.gov/pubmed/26266874
nmrlearner
News from NMR blogs
0
12-10-2015 01:09 AM
Polarization Transfer from Ligands Hyperpolarized by Dissolution Dynamic Nuclear Polarization for Screening in Drug Discovery
From The DNP-NMR Blog:
Polarization Transfer from Ligands Hyperpolarized by Dissolution Dynamic Nuclear Polarization for Screening in Drug Discovery
Min, H., G. Sekar, and C. Hilty, Polarization Transfer from Ligands Hyperpolarized by Dissolution Dynamic Nuclear Polarization for Screening in Drug Discovery. ChemMedChem, 2015. 10(9): p. 1559-63.
http://www.ncbi.nlm.nih.gov/pubmed/26315550
nmrlearner
News from NMR blogs
0
10-05-2015 07:08 PM
Effects of the electron polarization on dynamic nuclear polarization in solids
From The DNP-NMR Blog:
Effects of the electron polarization on dynamic nuclear polarization in solids
Hovav, Y., et al., Effects of the electron polarization on dynamic nuclear polarization in solids. Phys Chem Chem Phys, 2015. 17(8): p. 6053-65.
http://www.ncbi.nlm.nih.gov/pubmed/25640165
nmrlearner
News from NMR blogs
0
03-23-2015 08:22 PM
Cross Polarization for Dissolution Dynamic Nuclear Polarization
From The DNP-NMR Blog:
Cross Polarization for Dissolution Dynamic Nuclear Polarization
Batel, M., et al., Cross Polarization for Dissolution Dynamic Nuclear Polarization. Phys. Chem. Chem. Phys., 2014.
http://dx.doi.org/10.1039/C4CP02696A
nmrlearner
News from NMR blogs
0
08-22-2014 07:27 PM
Hyperpolarization of deuterated metabolites via remote cross-polarization and dissolution dynamic nuclear polarization
From The DNP-NMR Blog:
Hyperpolarization of deuterated metabolites via remote cross-polarization and dissolution dynamic nuclear polarization
Vuichoud, B., et al., Hyperpolarization of deuterated metabolites via remote cross-polarization and dissolution dynamic nuclear polarization. J Phys Chem B, 2014. 118(5): p. 1411-5.
http://www.ncbi.nlm.nih.gov/pubmed/24397585
Postdoctoral positions "high field ?MAS-DNP- NMR” and “Rapid melt DNP"
From The DNP-NMR Blog:
Postdoctoral positions "high field ?MAS-DNP- NMR” and “Rapid melt DNP"
Two postdoc positions for “DNP-enhanced NMR” both in the solid and liquid state are available immediately at the Solid State NMR group of the Institute of Molecules and Materials at the Radboud University of Nijmegen.
The solid NMR group at the Radboud University specializes in developing innovative technology to perform NMR spectroscopy on very small samples volumes both in the solid and in the liquid state. In the solid phase one can obtain ultrahigh proton decoupling fields (above 1...