Результаты исследований: Научные публикации в периодических изданиях › статья › Рецензирование
Ultrafast Single-Scan 2D NMR Spectroscopic Detection of a PHIP-Hyperpolarized Protease Inhibitor. / Kiryutin, Alexey S.; Sauer, Grit; Tietze, Daniel и др.
в: Chemistry - A European Journal, Том 25, № 16, 15.03.2019, стр. 4025-4030.Результаты исследований: Научные публикации в периодических изданиях › статья › Рецензирование
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TY - JOUR
T1 - Ultrafast Single-Scan 2D NMR Spectroscopic Detection of a PHIP-Hyperpolarized Protease Inhibitor
AU - Kiryutin, Alexey S.
AU - Sauer, Grit
AU - Tietze, Daniel
AU - Brodrecht, Martin
AU - Knecht, Stephan
AU - Yurkovskaya, Alexandra V.
AU - Ivanov, Konstantin L.
AU - Avrutina, Olga
AU - Kolmar, Harald
AU - Buntkowsky, Gerd
N1 - © 2019 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.
PY - 2019/3/15
Y1 - 2019/3/15
N2 - 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.
AB - 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.
KW - enzyme inhibitors
KW - hyperpolarization
KW - parahydrogen
KW - ultrafast 2D NMR
KW - Magnetic Resonance Spectroscopy/methods
KW - Protease Inhibitors/analysis
KW - Algorithms
KW - Imidazoles/chemistry
KW - Tyrosine/analogs & derivatives
KW - Molecular Structure
KW - Peptides, Cyclic/analysis
UR - http://www.scopus.com/inward/record.url?scp=85061915175&partnerID=8YFLogxK
U2 - 10.1002/chem.201900079
DO - 10.1002/chem.201900079
M3 - Article
C2 - 30698310
AN - SCOPUS:85061915175
VL - 25
SP - 4025
EP - 4030
JO - Chemistry - A European Journal
JF - Chemistry - A European Journal
SN - 0947-6539
IS - 16
ER -
ID: 18622780