Speeding Up 13C Direct Detection Biomolecular NMR Spectroscopy

被引:76
作者
Bermel, Wolfgang [3 ]
Bertini, Ivano [1 ,2 ]
Felli, Isabella C. [1 ,2 ]
Pierattelli, Roberta [1 ,2 ]
机构
[1] Univ Florence, CERM, I-50019 Florence, Italy
[2] Univ Florence, Dept Chem, I-50019 Florence, Italy
[3] Bruker BioSpin GmbH, D-76287 Rheinstetten, Germany
关键词
FAST MULTIDIMENSIONAL NMR; BACKBONE RESONANCE ASSIGNMENT; ALPHA DIRECT-DETECTION; PARAMAGNETIC PROTEINS; FOURIER-TRANSFORM; PROJECTION-RECONSTRUCTION; N-15; NMR; 2D NMR; HETERONUCLEAR; RESOLUTION;
D O I
10.1021/ja9058525
中图分类号
O6 [化学];
学科分类号
070301 [无机化学];
摘要
After the exploitation of H-1 polarization as a starting source for C-13 direct detection experiments, pulse sequences are designed which exploit the accelerated H-1 longitudinal relaxation to expedite C-13 direct detection experiments. We show here that 2D experiments based on C-13 direct detection on a 0.5 mM water sample of ubiquitin can be recorded in a few minutes and 3D experiments in a few hours. We also show that fast methods like nonuniform sampling can be easily implemented. As overall experimental time has always been a counter indication for the use of C-13 direct detection experiments, this research opens new avenues for the application of C-13 NMR to biological molecules.
引用
收藏
页码:15339 / 15345
页数:7
相关论文
共 89 条
[1]
Electronic Structure of the Ground and Excited States of the CuA Site by NMR Spectroscopy [J].
Abriata, Luciano A. ;
Ledesma, Gabriela N. ;
Pierattelli, Roberta ;
Vila, Alejandro J. .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2009, 131 (05) :1939-1946
[2]
Spin-state selection filters for the measurement of heteronuclear one-bond coupling constants [J].
Andersson, P ;
Weigelt, J ;
Otting, G .
JOURNAL OF BIOMOLECULAR NMR, 1998, 12 (03) :435-441
[3]
Rapid NMR data collection [J].
Atreya, HS ;
Szyperski, T .
NUCLEAR MAGNETIC RESONANCE OF BIOLOGICAL MACROMOLECULES, PART C, 2005, 394 :78-108
[4]
G-matrix Fourier transform NMR spectroscopy for complete protein resonance assignment [J].
Atreya, HS ;
Szyperski, T .
PROCEEDINGS OF THE NATIONAL ACADEMY OF SCIENCES OF THE UNITED STATES OF AMERICA, 2004, 101 (26) :9642-9647
[5]
Backbone and side-chains 1H, 13C and 15N NMR assignment of human β-parvalbumin [J].
Babini, E ;
Felli, IC ;
Lelli, M ;
Luchinat, C ;
Pierattelli, R .
JOURNAL OF BIOMOLECULAR NMR, 2005, 33 (02) :137-137
[6]
Assignment strategy for fast relaxing signals:: complete aminoacid identification in thulium substituted Calbindin D9K [J].
Balayssac, S ;
Jiménez, B ;
Piccioli, M .
JOURNAL OF BIOMOLECULAR NMR, 2006, 34 (02) :63-73
[7]
NMR OF PROTONS COUPLED TO C-13 NUCLEI ONLY [J].
BENDALL, MR ;
PEGG, DT ;
DODDRELL, DM ;
FIELD, J .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1981, 103 (04) :934-936
[8]
13C-detected protonless NMR spectroscopy of proteins in solution [J].
Bermel, W ;
Bertini, I ;
Felli, IC ;
Piccioli, M ;
Pierattelli, R .
PROGRESS IN NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY, 2006, 48 (01) :25-45
[9]
Protonless NMR experiments for sequence-specific assignment of backbone nuclei in unfolded proteins [J].
Bermel, W ;
Bertini, I ;
Felli, IC ;
Lee, YM ;
Luchinat, C ;
Pierattelli, R .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2006, 128 (12) :3918-3919
[10]
Novel 13C direct detection experiments, including extension to the third dimension, to perform the complete assignment of proteins [J].
Bermel, W ;
Bertini, I ;
Felli, IC ;
Kümmerle, R ;
Pierattelli, R .
JOURNAL OF MAGNETIC RESONANCE, 2006, 178 (01) :56-64