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Sensitivity-enhanced detection of non-labile proton and carbon NMR spectra on water resonances

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Abstract

Chemical exchange saturation transfer (CEST) experiments enhance the NMR signals of labile protons by continuously transferring these protons’ saturation to an abundant solvent pool like water. The present study expands these principles by fusing into these experiments homonuclear isotropic mixing sequences, enabling the water-enhanced detection of non-exchangeable species. Further opportunities are opened by the addition of coupling-mediated heteronuclear polarization transfers, which then impose on the water resonance a saturation stemming from non-labile heteronuclear species like 13C. To multiplex the ensuing experiments, these relayed approaches are combined with time-domain schemes involving multiple Ramsey-labeling experiments imparting the frequencies of the non-labile sites on the water resonance, via chemical exchange. 13C and 1H NMR spectra were detected in this fashion with about two-fold SNR amplification vis-à-vis conventionally detected spectroscopies. When combined with non-uniform sampling principles, this methodology thus becomes a sensitive alternative to detect non-exchangeable species in biomolecules. Still, multiple parameters including the scalar couplings and solvent exchange rates, will affect the efficiency and consequently the practicality of the overall experiment.

Graphical abstract: Sensitivity-enhanced detection of non-labile proton and carbon NMR spectra on water resonances

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Publication details

The article was received on 16 Oct 2017, accepted on 14 Nov 2017 and first published on 14 Nov 2017


Article type: Paper
DOI: 10.1039/C7CP07046B
Citation: Phys. Chem. Chem. Phys., 2018, Advance Article
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    Sensitivity-enhanced detection of non-labile proton and carbon NMR spectra on water resonances

    M. Novakovic, R. P. Martinho, G. L. Olsen, M. S. Lustig and L. Frydman, Phys. Chem. Chem. Phys., 2018, Advance Article , DOI: 10.1039/C7CP07046B

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