Ultrafast Single-Scan 2D-NMR Spectroscopic Detection of a PHIP-Hyperpolarized Protease Inhibitor

Ultrafast Single-Scan 2D-NMR Spectroscopic Detection of a PHIP-Hyperpolarized Protease Inhibitor Научная публикация

Журнал

Chemistry - A European Journal
ISSN: 0947-6539

Вых. Данные

Год: 2019, Том: 25, Номер: 16, Страницы: 4025-4030 Страниц : 6 DOI: 10.1002/chem.201900079

Авторы

Kiryutin Alexey S. ^1,2 , Sauer Grit ³ , Tietze Daniel ³ , Brodrecht Martin ³ , Knecht Stephan ³ , Yurkovskaya Alexandra V. ^1,2 , Ivanov Konstantin L. ^1,2 , Avrutina Olga ⁴ , Kolmar Harald ⁴ , Buntkowsky Gerd ³

Организации

1	International Tomography Center Institutskaya 3A, Novosibirsk (Russia)
2	Novosibirsk State University Pirogova 2, Novosibirsk, 630090 (Russia)
3	Eduard-Zintl-Institut fuer Anorganische und Physikalische Chemie Technische Universitaet Darmstadt Alarich-Weiss-Straße 8, 64287 Darmstadt (Germany)
4	Clemens-Schoepf-Institut fuer Organische Chemie und Biochemie Technische Universitaet Darmstadt Alarich-Weiss-Straße 4, 64287 Darmstadt (Germany)

Two-dimensional (2D) NMR is one of the most important spectroscopic tools for the investigation of biological macromolecules. However, owing to the low sensitivity of NMR it takes usually from several minutes to many hours to record such a spectrum. Here we show that a bioactive derivative of the sunflower trypsin inhibitor-1 (SFTI-1), a tetradecapeptide, can be detected by the combination of parahydrogen-induced polarization (PHIP) and ultrafast 2D-NMR spectroscopy (in the following abbreviated as 2D-NMR). The PHIP activity of the inhibitor was achieved by labeling with O-propargyl-L-tyrosine. In 1D-PHIP experiments an enhancement of approximately 1200 compared to normal 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.

Kiryutin A.S. , Sauer G. , Tietze D. , Brodrecht M. , Knecht S. , Yurkovskaya A.V. , Ivanov K.L. , Avrutina O. , Kolmar H. , Buntkowsky G.
Ultrafast Single-Scan 2D-NMR Spectroscopic Detection of a PHIP-Hyperpolarized Protease Inhibitor
Chemistry - A European Journal. 2019. V.25. N16. P.4025-4030. DOI: 10.1002/chem.201900079

Поступила в редакцию:	4 янв. 2019 г.
Принята к публикации:	30 янв. 2019 г.
Опубликована online:	30 янв. 2019 г.
Опубликована в печати:	17 февр. 2019 г.

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