Quantitative one- and two-dimensional 13C spectra of microcrystalline proteins with enhanced intensity

被引:17
作者
Purusottam, Rudra N. [1 ,2 ,3 ]
Bodenhausen, Geoffrey [1 ,2 ,3 ]
Tekely, Piotr [1 ,2 ,3 ]
机构
[1] Ecole Normale Super, Dept Chim, F-75005 Paris, France
[2] Univ Paris 06, F-75005 Paris, France
[3] CNRS, UMR 7203, Lab Biomol, F-75005 Paris, France
关键词
Solid-state NMR; PARIS rf-irradiation; Microcrystalline proteins; Quantitative C-13 spectra; Spin diffusion; Heteronuclear Overhauser enhancement; SOLID-STATE NMR; OVERHAUSER EFFECT MEASUREMENTS; NUCLEAR-MAGNETIC-RESONANCE; SURFACTANT SYSTEMS; SPECTROSCOPY; POLARIZATION; RELAXATION; FIELDS; WATER;
D O I
10.1007/s10858-013-9759-1
中图分类号
Q5 [生物化学]; Q7 [分子生物学];
学科分类号
071010 ; 081704 ;
摘要
We recorded quantitative, uniformly enhanced one- and two-dimensional C-13 spectra of labelled microcrystalline proteins. The approach takes advantage of efficient equilibration of magnetization by low-power proton irradiation using Phase Alternated Recoupling Irradiation Schemes and benefits simultaneously from uniform sensitivity enhancement due to efficient spin exchange that can overcome T-1(C-13) constraints and the presence of heteronuclear Overhauser effects.
引用
收藏
页码:11 / 19
页数:9
相关论文
共 21 条
[1]   HETERONUCLEAR OVERHAUSER EFFECT MEASUREMENTS IN SURFACTANT SYSTEMS .1. THE DIRECT ESTIMATION OF THE DISTANCE BETWEEN WATER AND THE MICELLAR SURFACE [J].
CANET, D ;
MAHIEU, N ;
TEKELY, P .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1992, 114 (15) :6190-6194
[2]   Impact of selective excitation on carbon longitudinal relaxation: Towards fast solid-state NMR techniques [J].
Giffard, Mathilde ;
Bardet, Michel ;
Bersch, Beate ;
Coves, Jacques ;
Hediger, Sabine .
JOURNAL OF MAGNETIC RESONANCE, 2009, 200 (01) :153-160
[3]   Observation of heteronuclear overhauser effects confirms the 15N-1H dipolar relaxation mechanism in a crystalline protein [J].
Giraud, Nicolas ;
Sein, Julien ;
Pintacuda, Guido ;
Bockmann, Anja ;
Lesage, Anne ;
Blackledge, Martin ;
Emsley, Lyndon .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2006, 128 (38) :12398-12399
[4]   Probing Structural and Motional Features of the C-Terminal Part of the Human Centrin 2/P17-XPC Microcrystalline Complex by Solid-State NMR Spectroscopy [J].
Herbert-Pucheta, Jose-Enrique ;
Chan-Huot, Monique ;
Duma, Luminita ;
Abergel, Daniel ;
Bodenhausen, Geoffrey ;
Assairi, Liliane ;
Bouquit, Yves ;
Charbonnier, Jean-Baptiste ;
Tekely, Piotr .
JOURNAL OF PHYSICAL CHEMISTRY B, 2012, 116 (50) :14581-14591
[5]   Restoring symmetry in two-dimensional solid-state NMR correlation spectra [J].
Herbert-Pucheta, Jose-Enrique ;
Pelupessy, Philippe ;
Bodenhausen, Geoffrey ;
Tekely, Piotr .
CHEMICAL PHYSICS LETTERS, 2012, 539 :245-251
[6]   Disentangling Crystallographic Inequivalence and Crystallographic Forms of L-Arginine by One- and Two-Dimensional Solid-State NMR Spectroscopy [J].
Herbert-Pucheta, Jose-Enrique ;
Colaux, Henri ;
Bodenhausen, Geoffrey ;
Tekely, Piotr .
JOURNAL OF PHYSICAL CHEMISTRY B, 2011, 115 (51) :15415-15421
[7]   Breaking the T1 Constraint for Quantitative Measurement in Magic Angle Spinning Solid-State NMR Spectroscopy [J].
Hou, Guangjin ;
Ding, Shangwu ;
Zhang, Limin ;
Deng, Feng .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2010, 132 (16) :5538-+
[8]   13C nuclear overhauser polarization-magic-angle spinning nuclear magnetic resonance spectroscopy in uniformly 13C-labeled solid proteins [J].
Katoh, E ;
Takegoshi, K ;
Terao, T .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2004, 126 (11) :3653-3657
[9]   Investigation of dipolar-mediated water-protein interactions in microcrystalline Crh by solid-state NMR spectroscopy [J].
Lesage, Anne ;
Emsley, Lyndon ;
Penin, Francois ;
Bockmann, Anja .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2006, 128 (25) :8246-8255
[10]   ANISOTROPIC BEHAVIOR OF THE C-13 NUCLEAR-SPIN DYNAMICS IN A SINGLE-CRYSTAL OF L-ALANINE [J].
NAITO, A ;
MCDOWELL, CA .
JOURNAL OF CHEMICAL PHYSICS, 1986, 84 (08) :4181-4186