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J Magn Reson. 2017 Dec;285:26-36. doi: 10.1016/j.jmr.2017.10.007. Epub 2017 Oct 16.

A highly versatile automatized setup for quantitative measurements of PHIP enhancements.

Author information

1
International Tomography Center, Institutskaya 3A, Novosibirsk 630090, Russia; Novosibirsk State University, Pirogova 2, Novosibirsk 630090, Russia.
2
Technische Universität Darmstadt, Eduard-Zintl-Institut für Anorganische und Physikalische Chemie, Alarich-Weiss-Straße 8, Darmstadt 64287, Germany.
3
Technische Universität Darmstadt, Eduard-Zintl-Institut für Anorganische und Physikalische Chemie, Alarich-Weiss-Straße 8, Darmstadt 64287, Germany. Electronic address: gerd.buntkowsky@chemie.tu-darmstadt.de.

Abstract

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.

KEYWORDS:

Gas-dissolution; Hyperpolarization; Kinetics; Parahydrogen Induced Polarization

PMID:
29073504
DOI:
10.1016/j.jmr.2017.10.007

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