Herr, Kevin ; Fleckenstein, Max ; Brodrecht, Martin ; Höfler, Mark V. ; Heise, Henrike ; Aussenac, Fabien ; Gutmann, Torsten ; Reggelin, Michael ; Buntkowsky, Gerd (2021)
A novel strategy for site selective spin-labeling to investigate bioactive entities by DNP and EPR spectroscopy.
In: Scientific Reports, 11 (1)
doi: 10.1038/s41598-021-92975-6
Artikel, Bibliographie
Dies ist die neueste Version dieses Eintrags.
Kurzbeschreibung (Abstract)
A novel specific spin-labeling strategy for bioactive molecules is presented for eptifibatide (integrilin) an antiplatelet aggregation inhibitor, which derives from the venom of certain rattlesnakes. By specifically labeling the disulfide bridge this molecule becomes accessible for analytical techniques such as Electron Paramagnetic Resonance (EPR) and solid state Dynamic Nuclear Polarization (DNP). The necessary spin-label was synthesized and inserted into the disulfide bridge of eptifibatide via reductive followed by insertion by a double Michael addition under physiological conditions. This procedure is universally applicable for disulfide containing biomolecules and is expected to preserve their tertiary structure with minimal change due to the small size of the label and restoring of the previous disulfide connection. HPLC and MS analysis show the successful introduction of the spin label and EPR spectroscopy confirms its activity. DNP-enhanced solid state NMR experiments show signal enhancement factors of up to 19 in ¹³C CP MAS experiments which corresponds to time saving factors of up to 361. This clearly shows the high potential of our new spin labeling strategy for the introduction of site selective radical spin labels into biomolecules and biosolids without compromising its conformational integrity for structural investigations employing solid-state DNP or advanced EPR techniques.
| Typ des Eintrags: | Artikel |
|---|---|
| Erschienen: | 2021 |
| Autor(en): | Herr, Kevin ; Fleckenstein, Max ; Brodrecht, Martin ; Höfler, Mark V. ; Heise, Henrike ; Aussenac, Fabien ; Gutmann, Torsten ; Reggelin, Michael ; Buntkowsky, Gerd |
| Art des Eintrags: | Bibliographie |
| Titel: | A novel strategy for site selective spin-labeling to investigate bioactive entities by DNP and EPR spectroscopy |
| Sprache: | Englisch |
| Publikationsjahr: | 2021 |
| Ort: | Darmstadt |
| Verlag: | Springer Nature |
| Titel der Zeitschrift, Zeitung oder Schriftenreihe: | Scientific Reports |
| Jahrgang/Volume einer Zeitschrift: | 11 |
| (Heft-)Nummer: | 1 |
| Kollation: | 12 Seiten |
| DOI: | 10.1038/s41598-021-92975-6 |
| Zugehörige Links: | |
| Kurzbeschreibung (Abstract): | A novel specific spin-labeling strategy for bioactive molecules is presented for eptifibatide (integrilin) an antiplatelet aggregation inhibitor, which derives from the venom of certain rattlesnakes. By specifically labeling the disulfide bridge this molecule becomes accessible for analytical techniques such as Electron Paramagnetic Resonance (EPR) and solid state Dynamic Nuclear Polarization (DNP). The necessary spin-label was synthesized and inserted into the disulfide bridge of eptifibatide via reductive followed by insertion by a double Michael addition under physiological conditions. This procedure is universally applicable for disulfide containing biomolecules and is expected to preserve their tertiary structure with minimal change due to the small size of the label and restoring of the previous disulfide connection. HPLC and MS analysis show the successful introduction of the spin label and EPR spectroscopy confirms its activity. DNP-enhanced solid state NMR experiments show signal enhancement factors of up to 19 in ¹³C CP MAS experiments which corresponds to time saving factors of up to 361. This clearly shows the high potential of our new spin labeling strategy for the introduction of site selective radical spin labels into biomolecules and biosolids without compromising its conformational integrity for structural investigations employing solid-state DNP or advanced EPR techniques. |
| Freie Schlagworte: | Biophysical chemistry, Chemical physics, Synthetic chemistry methodology |
| ID-Nummer: | 13714 |
| Sachgruppe der Dewey Dezimalklassifikatin (DDC): | 500 Naturwissenschaften und Mathematik > 530 Physik 500 Naturwissenschaften und Mathematik > 540 Chemie |
| Fachbereich(e)/-gebiet(e): | 07 Fachbereich Chemie 07 Fachbereich Chemie > Clemens-Schöpf-Institut 07 Fachbereich Chemie > Eduard Zintl-Institut 07 Fachbereich Chemie > Clemens-Schöpf-Institut > Fachgebiet Organische Chemie 07 Fachbereich Chemie > Eduard Zintl-Institut > Fachgebiet Physikalische Chemie |
| Hinterlegungsdatum: | 02 Aug 2024 12:54 |
| Letzte Änderung: | 02 Aug 2024 12:54 |
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| Suche nach Titel in: | TUfind oder in Google |
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A novel strategy for site selective spin-labeling to investigate bioactive entities by DNP and EPR spectroscopy. (deposited 13 Jul 2023 12:55)
- A novel strategy for site selective spin-labeling to investigate bioactive entities by DNP and EPR spectroscopy. (deposited 02 Aug 2024 12:54) [Gegenwärtig angezeigt]
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