Journal
CHEMISTRY-A EUROPEAN JOURNAL
Volume 25, Issue 16, Pages 4025-4030Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/chem.201900079
Keywords
enzyme inhibitors; hyperpolarization; parahydrogen; ultrafast 2D NMR
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Funding
- Deutsche Forschungsgemeinschaft DFG [Bu-911-22-1]
- Russian Science Foundation [19-43-04116]
- state of Hesse
- Russian Science Foundation [19-43-04116] Funding Source: Russian Science Foundation
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Two-dimensional NMR spectroscopy is one of the most important spectroscopic tools for the investigation of biological macromolecules. However, due to the low sensitivity of NMR spectroscopy, it takes usually from several minutes to many hours to record such spectra. Here, the possibility of detecting a bioactive derivative of the sunflower trypsin inhibitor-1 (SFTI-1), a tetradecapeptide, by combining parahydrogen-induced polarization (PHIP) and ultrafast 2D NMR spectroscopy is shown. The PHIP activity of the inhibitor was achieved by labeling with O-propargyl-l-tyrosine. In 1D PHIP experiments a signal enhancement of a factor of approximately 1200 compared to standard NMR was found. This enhancement permits measurement of 2D NMR correlation spectra of low-concentrated SFTI-1 in less than 10 seconds, employing ultrafast single-scan 2D NMR detection. As experimental examples PHIP-assisted ultrafast single-scan TOCSY spectra of SFTI-1 are shown.
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