2H-DNP-enhanced 2H-13C solid-state NMR correlation spectroscopy.
Perdeuteration of biological macromolecules for magic angle spinning solid-state NMR spectroscopy can yield high-resolution (2)H-(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 (2)H-(13)C correlation spectra with a signal enhancement of epsilon > or = 700 compared to a spectrum recorded with microwaves off and otherwise identical conditions. To our knowledge, this is the first time that (2)H-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 (2)H-(13)C correlation spectra of U-[(2)H, (13)C] proline.
Maly
Thorsten
T
Francis Bitter Magnet Laboratory and Department of Chemistry, Cambridge, MA 02139, USA.
Andreas
Loren B
LB
Smith
Albert A
AA
Griffin
Robert G
RG
D002247:Carbon Isotopes / Q000737:chemistry; D003497:Cyclic N-Oxides / Q000737:chemistry; D003903:Deuterium / Q000737:chemistry; D019906:Nuclear Magnetic Resonance, Biomolecular / Q000379:methods*; D011392:Proline / Q000737:chemistry; D020005:Propanols / Q000737:chemistry
C521769:1-(TEMPO-4-oxy)-3-(TEMPO-4-amino)propan-2-ol; D002247:Carbon Isotopes; D003497:Cyclic N-Oxides; D020005:Propanols; D011392:Proline; D003903:Deuterium
Appl Magn Reson. 2008 Aug;34(3-4):237-263
19194532
J Am Chem Soc. 2006 Sep 6;128(35):11385-90
16939261
J Biomol NMR. 2005 Mar;31(3):217-30
15803395
J Am Chem Soc. 2006 Aug 23;128(33):10840-6
16910679
Chemphyschem. 2010 Apr 6;11(5):999-1001
20169604
J Am Chem Soc. 2005 Jan 12;127(1):397-404
15631490
J Magn Reson. 2005 Feb;172(2):254-67
15649753
J Magn Reson. 2009 Jun;198(2):261-70
19356957
Proc Natl Acad Sci U S A. 2003 Sep 2;100(18):10158-63
12930897
J Magn Reson. 2008 Sep;194(1):16-24
18571955
Top Curr Chem. 2005;246:15-31
22160287
J Am Chem Soc. 2006 Oct 4;128(39):12620-1
17002335
Nature. 2008 Jun 12;453(7197):940-3
18509335
Proc Natl Acad Sci U S A. 2009 Jun 9;106(23):9244-9
19474298
J Chem Phys. 2008 Feb 7;128(5):052211
18266416
J Magn Reson. 1999 Jun;138(2):232-43
10341127
IEEE Trans Plasma Sci IEEE Nucl Plasma Sci Soc. 2010 Jun 1;38(6):1150-1160
21243088
Angew Chem Int Ed Engl. 2009;48(27):4996-5000
19492374
J Magn Reson. 2006 Dec;183(2):303-7
17027306
Phys Rev Lett. 1993 Nov 22;71(21):3561-3564
10055008
J Am Chem Soc. 2009 Jan 14;131(1):2-3
19072045
Chemphyschem. 2004 Jul 19;5(7):966-74
15298382
J Chem Phys. 2008 Feb 7;128(5):052302
18266419
J Magn Reson. 2003 Jul;163(1):105-13
12852913
J Am Chem Soc. 2004 Sep 8;126(35):10844-5
15339160
Annu Rev Biophys. 2009;38:385-403
19245337
J Am Chem Soc. 2007 Sep 26;129(38):11791-801
17725352
J Magn Reson. 2008 Jan;190(1):135-41
17910927
J Org Chem. 2002 Jul 12;67(14):4635-9
12098269
Phys Chem Chem Phys. 2010 Jun 14;12(22):5861-7
20454732