TY - JOUR

T1 - A highly versatile automatized setup for quantitative measurements of PHIP enhancements

AU - Kiryutin, Alexey S.

AU - Sauer, Grit

AU - Hadjiali, Sara

AU - Yurkovskaya, Alexandra V.

AU - Breitzke, Hergen

AU - Buntkowsky, Gerd

N1 - Copyright © 2017 Elsevier Inc. All rights reserved.

PY - 2017/12/1

Y1 - 2017/12/1

N2 - 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.

AB - 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.

KW - Gas-dissolution

KW - Hyperpolarization

KW - Kinetics

KW - Parahydrogen Induced Polarization

KW - SIGNAL ENHANCEMENT

KW - CONTRAST AGENTS

KW - NUCLEAR-MAGNETIC-RESONANCE

KW - SPIN HYPERPOLARIZATION

KW - REVERSIBLE EXCHANGE

KW - HYDROGEN

KW - SPECTROSCOPY

KW - SABRE

KW - PARAHYDROGEN-INDUCED POLARIZATION

KW - STATE NMR CHARACTERIZATION

UR - http://www.scopus.com/inward/record.url?scp=85032871189&partnerID=8YFLogxK

U2 - 10.1016/j.jmr.2017.10.007

DO - 10.1016/j.jmr.2017.10.007

M3 - Article

C2 - 29073504

AN - SCOPUS:85032871189

VL - 285

SP - 26

EP - 36

JO - Journal of Magnetic Resonance

JF - Journal of Magnetic Resonance

SN - 1090-7807

ER -