The design and application of a versatile and inexpensive experimental extension to NMR spectrometers is described that allows to carry out highly reproducible PHIP experiments directly in the NMR sample tube, i.e. under PASADENA condition, followed by the detection of the NMR spectra of hyperpolarized products with high spectral resolution. Employing this high resolution it is feasible to study kinetic processes in the solution with high accuracy. As a practical example the dissolution of hydrogen gas in the liquid and the PHIP kinetics during the hydrogenation reaction of Fmoc-O-propargyl-l-tyrosine in acetone-d6 are monitored. The timing of the setup is fully controlled by the pulse-programmer of the NMR spectrometer. By flushing with an inert gas it is possible to efficiently quench the hydrogenation reaction in a controlled fashion and to detect the relaxation of hyperpolarization without a background reaction. The proposed design makes it possible to carry out PHIP experiments in an automatic mode and reliably determine the enhancement of polarized signals.
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[NMR paper] Rapid Quantitative Measurements of Paramagnetic Relaxation Enhancements in Cu(II)-Tagged Proteins by Proton-Detected Solid-State NMR Spectroscopy.
Rapid Quantitative Measurements of Paramagnetic Relaxation Enhancements in Cu(II)-Tagged Proteins by Proton-Detected Solid-State NMR Spectroscopy.
Related Articles Rapid Quantitative Measurements of Paramagnetic Relaxation Enhancements in Cu(II)-Tagged Proteins by Proton-Detected Solid-State NMR Spectroscopy.
J Phys Chem Lett. 2017 Nov 17;:
Authors: Mukhopadhyay D, Nadaud PS, Shannon MD, Jaroniec CP
Abstract
We demonstrate rapid quantitative measurements of site-resolved paramagnetic relaxation enhancements (PREs), which are a...
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11-19-2017 05:41 AM
[NMR paper] Disassembly/reassembly strategy for the production of highly pure GroEL, a tetradecameric supramolecular machine, suitable for quantitative NMR, EPR and mutational studies.
Disassembly/reassembly strategy for the production of highly pure GroEL, a tetradecameric supramolecular machine, suitable for quantitative NMR, EPR and mutational studies.
Related Articles Disassembly/reassembly strategy for the production of highly pure GroEL, a tetradecameric supramolecular machine, suitable for quantitative NMR, EPR and mutational studies.
Protein Expr Purif. 2017 Sep 22;:
Authors: Wälti MA, Clore GM
Abstract
GroEL, a prototypical member of the chaperonin class of chaperones, is a large supramocular...
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09-28-2017 07:57 PM
[NMR paper] Self-assembled Oligopeptide as a Versatile NMR Alignment Medium for the Measurements of Residual Dipolar Couplings in Methanol
Self-assembled Oligopeptide as a Versatile NMR Alignment Medium for the Measurements of Residual Dipolar Couplings in Methanol
Residual dipolar coupling (RDC) constitutes a powerful structural parameter for the determination of constitution, conformation and configuration of organic molecules. Here, we report the first liquid crystalline based orientating medium that is compatible with MeOH, thus enabling RDC acquisitions of a wide range of intermediate to polar organic molecules. The liquid crystals were produced by the self-assembled oligopeptide nanotubes (AAKLVFF), which are stable...
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08-23-2017 05:25 PM
Toward Quantitative Measurements of Enzyme Kinetics by Dissolution Dynamic Nuclear Polarization
From The DNP-NMR Blog:
Toward Quantitative Measurements of Enzyme Kinetics by Dissolution Dynamic Nuclear Polarization
Miclet E, Abergel D, Bornet A, Milani J, Jannin S, Bodenhausen G. Toward Quantitative Measurements of Enzyme Kinetics by Dissolution Dynamic Nuclear Polarization. The Journal of Physical Chemistry Letters. 2014;5(19):3290-5.
http://dx.doi.org/10.1021/jz501411d
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06-03-2015 11:04 PM
Quantitative Trace Analysis of Complex Mixtures Using SABRE Hyperpolarization
From The DNP-NMR Blog:
Quantitative Trace Analysis of Complex Mixtures Using SABRE Hyperpolarization
Eshuis, N., et al., Quantitative Trace Analysis of Complex Mixtures Using SABRE Hyperpolarization. Angew Chem Int Ed Engl, 2014: p. n/a-n/a.
http://www.ncbi.nlm.nih.gov/pubmed/25469822
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01-12-2015 11:31 PM
[Question from NMRWiki Q&A forum] PHIP experiments
PHIP experiments
Dear all! I am struggling with some density matrices in PHIP experiments. I understand why the density matrix before hydrogenation reaction is I dot S But why afterwards (in PASADENA exp. for example) the density matrix is just IzSz? And in ALTADENA is IzSz-0.5(Iz-Sz)? Thank you!
Check if somebody has answered this question on NMRWiki QA forum
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11-28-2013 05:18 PM
Postdoc NMR - PHIP
Postdoc NMR - PHIP
Currently we are looking for a post-doctoral researcher in the area of para-hydrogen induced hyperpolarisation (PHIP). The position aims specifically for development of the PHIP methodology and instrumentation for screening, biomarker research and/or molecular diagnostics. The post-doc (initially 2 yrs; extension is possible) should have a background in (Physical) Chemistry and/or Analytical Sciences with knowledge of MR spectroscopy (e.g. NMR or MRI) and an interest in methodological development and instrumentation. Expertise in para-hydrogen based NMR technology is an...
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04-06-2012 01:23 AM
Conformational analysis by quantitative NOE measurements of the β-proton pairs across individual disulfide bonds in proteins
Conformational analysis by quantitative NOE measurements of the β-proton pairs across individual disulfide bonds in proteins
Abstract NOEs between the β-protons of cysteine residues across disulfide bonds in proteins provide direct information on the connectivities and conformations of these important cross-links, which are otherwise difficult to investigate. With conventional -proteins, however, fast spin diffusion processes mediated by strong dipolar interactions between geminal β-protons prohibit the quantitative measurements and thus the analyses of long-range NOEs across...
A highly versatile automatized setup for quantitative measurements of PHIP enhancements #SABRE #NMR
Linear Mode
