[superscript 2]H-DNP-enhanced [superscript 2]H-[superscript 13]C solid-state NMR correlation spectroscopy
Perdeuteration of biological macromolecules for magic angle spinning solid-state NMR spectroscopy can yield high-resolution [superscript 2]H–[superscript 13]C correlation spectra and the method is therefore of great interest for the structural biology community. Here we demonstrate that the combinat...
| Main Authors: | , , , |
|---|---|
| Other Authors: | |
| Format: | Article |
| Language: | en_US |
| Published: |
Royal Society of Chemistry, The
2012
|
| Online Access: | http://hdl.handle.net/1721.1/74630 https://orcid.org/0000-0003-1589-832X |
| _version_ | 1826209321324642304 |
|---|---|
| author | Maly, Thorsten Andreas, Loren Griffin, Robert Guy Smith, Albert A. |
| author2 | Massachusetts Institute of Technology. Department of Chemistry |
| author_facet | Massachusetts Institute of Technology. Department of Chemistry Maly, Thorsten Andreas, Loren Griffin, Robert Guy Smith, Albert A. |
| author_sort | Maly, Thorsten |
| collection | MIT |
| description | Perdeuteration of biological macromolecules for magic angle spinning solid-state NMR spectroscopy can yield high-resolution [superscript 2]H–[superscript 13]C correlation spectra and the method is therefore of great interest for the structural biology community. Here we demonstrate that the combination of sample deuteration and dynamic nuclear polarization yields resolved [superscript 2]H–[superscript 13]C correlation spectra with a signal enhancement of ε ≥ 700 compared to a spectrum recorded with microwaves off and otherwise identical conditions. To our knowledge, this is the first time that [superscript 2]2H-DNP has been employed to enhance MAS-NMR spectra of a biologically relevant system. The DNP process is studied using several polarizing agents and the technique is applied to obtain [superscript 2]H–[superscript 13]C correlation spectra of U-[[superscript 2]H, [superscript 13]C] proline. |
| first_indexed | 2024-09-23T14:21:01Z |
| format | Article |
| id | mit-1721.1/74630 |
| institution | Massachusetts Institute of Technology |
| language | en_US |
| last_indexed | 2024-09-23T14:21:01Z |
| publishDate | 2012 |
| publisher | Royal Society of Chemistry, The |
| record_format | dspace |
| spelling | mit-1721.1/746302022-09-29T08:51:22Z [superscript 2]H-DNP-enhanced [superscript 2]H-[superscript 13]C solid-state NMR correlation spectroscopy Maly, Thorsten Andreas, Loren Griffin, Robert Guy Smith, Albert A. Massachusetts Institute of Technology. Department of Chemistry Francis Bitter Magnet Laboratory (Massachusetts Institute of Technology) Griffin, Robert G. Maly, Thorsten Andreas, Loren Smith, Albert Andrew Griffin, Robert Guy Perdeuteration of biological macromolecules for magic angle spinning solid-state NMR spectroscopy can yield high-resolution [superscript 2]H–[superscript 13]C correlation spectra and the method is therefore of great interest for the structural biology community. Here we demonstrate that the combination of sample deuteration and dynamic nuclear polarization yields resolved [superscript 2]H–[superscript 13]C correlation spectra with a signal enhancement of ε ≥ 700 compared to a spectrum recorded with microwaves off and otherwise identical conditions. To our knowledge, this is the first time that [superscript 2]2H-DNP has been employed to enhance MAS-NMR spectra of a biologically relevant system. The DNP process is studied using several polarizing agents and the technique is applied to obtain [superscript 2]H–[superscript 13]C correlation spectra of U-[[superscript 2]H, [superscript 13]C] proline. National Institutes of Health (U.S.) (Grant EB002084) National Institutes of Health (U.S.) (Grant EB002026) German Research Foundation. Research Fellowship National Science Foundation (U.S.). Graduate Research Fellowship Program 2012-11-13T16:50:29Z 2012-11-13T16:50:29Z 2010-05 2010-03 Article http://purl.org/eprint/type/JournalArticle 1463-9076 1463-9084 http://hdl.handle.net/1721.1/74630 Maly, Thorsten et al. “2H-DNP-enhanced 2H–13C Solid-state NMR Correlation Spectroscopy.” Physical Chemistry Chemical Physics 12.22 (2010): 5872. https://orcid.org/0000-0003-1589-832X en_US http://dx.doi.org/ 10.1039/c003705b Physical Chemistry Chemical Physics Creative Commons Attribution-Noncommercial-Share Alike 3.0 http://creativecommons.org/licenses/by-nc-sa/3.0/ application/pdf Royal Society of Chemistry, The Prof. Griffin via Erja Kajosalo |
| spellingShingle | Maly, Thorsten Andreas, Loren Griffin, Robert Guy Smith, Albert A. [superscript 2]H-DNP-enhanced [superscript 2]H-[superscript 13]C solid-state NMR correlation spectroscopy |
| title | [superscript 2]H-DNP-enhanced [superscript 2]H-[superscript 13]C solid-state NMR correlation spectroscopy |
| title_full | [superscript 2]H-DNP-enhanced [superscript 2]H-[superscript 13]C solid-state NMR correlation spectroscopy |
| title_fullStr | [superscript 2]H-DNP-enhanced [superscript 2]H-[superscript 13]C solid-state NMR correlation spectroscopy |
| title_full_unstemmed | [superscript 2]H-DNP-enhanced [superscript 2]H-[superscript 13]C solid-state NMR correlation spectroscopy |
| title_short | [superscript 2]H-DNP-enhanced [superscript 2]H-[superscript 13]C solid-state NMR correlation spectroscopy |
| title_sort | superscript 2 h dnp enhanced superscript 2 h superscript 13 c solid state nmr correlation spectroscopy |
| url | http://hdl.handle.net/1721.1/74630 https://orcid.org/0000-0003-1589-832X |
| work_keys_str_mv | AT malythorsten superscript2hdnpenhancedsuperscript2hsuperscript13csolidstatenmrcorrelationspectroscopy AT andreasloren superscript2hdnpenhancedsuperscript2hsuperscript13csolidstatenmrcorrelationspectroscopy AT griffinrobertguy superscript2hdnpenhancedsuperscript2hsuperscript13csolidstatenmrcorrelationspectroscopy AT smithalberta superscript2hdnpenhancedsuperscript2hsuperscript13csolidstatenmrcorrelationspectroscopy |