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Issue 14, 2018
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SABRE hyperpolarization enables high-sensitivity 1H and 13C benchtop NMR spectroscopy

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Abstract

Benchtop NMR spectrometers operating with low magnetic fields of 1–2 T at sub-ppm resolution show great promise as analytical platforms that can be used outside the traditional laboratory environment for industrial process monitoring. One current limitation that reduces the uptake of benchtop NMR is associated with the detection fields’ reduced sensitivity. Here we demonstrate how para-hydrogen (p-H2) based signal amplification by reversible exchange (SABRE), a simple to achieve hyperpolarization technique, enhances agent detectability within the environment of a benchtop (1 T) NMR spectrometer so that informative 1H and 13C NMR spectra can be readily recorded for low-concentration analytes. SABRE-derived 1H NMR signal enhancements of up to 17 000-fold, corresponding to 1H polarization levels of P = 5.9%, were achieved for 26 mM pyridine in d4-methanol in a matter of seconds. Comparable enhancement levels can be achieved in both deuterated and protio solvents but now the SABRE-enhanced analyte signals dominate due to the comparatively weak thermally-polarized solvent response. The SABRE approach also enables the acquisition of 13C NMR spectra of analytes at natural isotopic abundance in a single scan as evidenced by hyperpolarized 13C NMR spectra of tens of millimolar concentrations of 4-methylpyridine. Now the associated signal enhancement factors are up to 45 500 fold (P = 4.0%) and achieved in just 15 s. Integration of an automated SABRE polarization system with the benchtop NMR spectrometer framework produces renewable and reproducible NMR signal enhancements that can be exploited for the collection of multi-dimensional NMR spectra, exemplified here by a SABRE-enhanced 2D COSY NMR spectrum.

Graphical abstract: SABRE hyperpolarization enables high-sensitivity 1H and 13C benchtop NMR spectroscopy

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Publication details

The article was received on 29 Mar 2018, accepted on 01 Jun 2018 and first published on 19 Jun 2018


Article type: Paper
DOI: 10.1039/C8AN00596F
Citation: Analyst, 2018,143, 3442-3450
  • Open access: Creative Commons BY license
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    SABRE hyperpolarization enables high-sensitivity 1H and 13C benchtop NMR spectroscopy

    P. M. Richardson, A. J. Parrott, O. Semenova, A. Nordon, S. B. Duckett and M. E. Halse, Analyst, 2018, 143, 3442
    DOI: 10.1039/C8AN00596F

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