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
Article, Bibliographie
This is the latest version of this item.
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.
| Item Type: | Article |
|---|---|
| Erschienen: | 2021 |
| Creators: | Herr, Kevin ; Fleckenstein, Max ; Brodrecht, Martin ; Höfler, Mark V. ; Heise, Henrike ; Aussenac, Fabien ; Gutmann, Torsten ; Reggelin, Michael ; Buntkowsky, Gerd |
| Type of entry: | Bibliographie |
| Title: | A novel strategy for site selective spin-labeling to investigate bioactive entities by DNP and EPR spectroscopy |
| Language: | English |
| Date: | 2021 |
| Place of Publication: | Darmstadt |
| Publisher: | Springer Nature |
| Journal or Publication Title: | Scientific Reports |
| Volume of the journal: | 11 |
| Issue Number: | 1 |
| Collation: | 12 Seiten |
| DOI: | 10.1038/s41598-021-92975-6 |
| Corresponding Links: | |
| 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. |
| Uncontrolled Keywords: | Biophysical chemistry, Chemical physics, Synthetic chemistry methodology |
| Identification Number: | 13714 |
| Classification DDC: | 500 Science and mathematics > 530 Physics 500 Science and mathematics > 540 Chemistry |
| Divisions: | 07 Department of Chemistry 07 Department of Chemistry > Clemens-Schöpf-Institut 07 Department of Chemistry > Eduard Zintl-Institut 07 Department of Chemistry > Clemens-Schöpf-Institut > Organ Chemistry 07 Department of Chemistry > Eduard Zintl-Institut > Physical Chemistry |
| Date Deposited: | 02 Aug 2024 12:54 |
| Last Modified: | 02 Aug 2024 12:54 |
| PPN: | |
| Export: | |
| Suche nach Titel in: | TUfind oder in Google |
Available Versions of this Item
-
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) [Currently Displayed]
 |
Send an inquiry |
Options (only for editors)
 |
Show editorial Details |
Drucken
Impressum