High resolution 13C DOSY: The DEPTSE experiment

被引:28
作者
Botana, Adolfo [1 ]
Howe, Peter W. A. [2 ]
Caer, Valerie [2 ,3 ]
Morris, Gareth A. [1 ]
Nilsson, Mathias [1 ]
机构
[1] Univ Manchester, Sch Chem, Manchester M13 9PL, Lancs, England
[2] Syngenta Ltd, Analyt Sci, Jealotts Hill Res Ctr, Bracknell RG42 6EY, Berks, England
[3] Syngenta Crop Protect AG, CH-4058 Basel, Switzerland
基金
英国工程与自然科学研究理事会;
关键词
DOSY; Polarization transfer; Diffusion; Carbon; Mixture analysis; Spin echo; DEPT; DEPTSE; DIFFUSION-ORDERED SPECTROSCOPY; IMPROVING PULSE SEQUENCES; LEAST-SQUARES ANALYSIS; SPECTRAL DATA SETS; NMR-SPECTROSCOPY; PGSE NMR; 3D DOSY; 2D; DECRA; COEFFICIENTS;
D O I
10.1016/j.jmr.2011.03.016
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
High Resolution Diffusion-ordered Spectroscopy (HR-DOSY) is a valuable tool for mixture analysis by NMR. it separates the signals from different components according to their diffusion behavior, and can provide exquisite diffusion resolution when there is no signal overlap. In HR-DOSY experiments on H-1 (by far the most common nucleus used for DOSY) there is frequent signal overlap that confuses interpretation. In contrast, a C-13 spectrum usually has little overlap, and is in this respect a much better option for a DOSY experiment. The low signal-to-noise ratio is a critical limiting factor, but with recent technical advances such as cryogenic probes this problem is now less acute. The most widely-used pulse sequences for C-13 DOSY perform diffusion encoding with H-1, using a stimulated echo in which half of the signal is lost. This signal loss can be avoided by encoding diffusion with C-13 in a spin echo experiment such as the DEPTSE pulse sequence described here. (C) 2011 Elsevier Inc. All rights reserved.
引用
收藏
页码:25 / 29
页数:5
相关论文
共 61 条
[1]   Pure Shift 1H NMR: A Resolution of the Resolution Problem? [J].
Aguilar, Juan A. ;
Faulkner, Stephen ;
Nilsson, Mathias ;
Morris, Gareth A. .
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION, 2010, 49 (23) :3901-3903
[2]   Enhanced 13C PFG NMR for the study of hydrodynamic dispersion in porous media [J].
Akpa, Belinda S. ;
Holland, Daniel J. ;
Sederman, Andrew J. ;
Johns, Michael L. ;
Gladden, Lynn F. .
JOURNAL OF MAGNETIC RESONANCE, 2007, 186 (01) :160-165
[3]   The use of PGSE NMR and DECRA for determining polymer composition [J].
Antalek, B ;
Hewitt, JM ;
Windig, W ;
Yacobucci, PD ;
Mourey, T ;
Le, K .
MAGNETIC RESONANCE IN CHEMISTRY, 2002, 40 (SPEC. ISS.) :S60-S71
[4]   A three-dimensional DOSY-HMQC experiment for the high-resolution analysis of complex mixtures [J].
Barjat, H ;
Morris, GA ;
Swanson, AG .
JOURNAL OF MAGNETIC RESONANCE, 1998, 131 (01) :131-138
[5]   HIGH-RESOLUTION DIFFUSION-ORDERED 2D SPECTROSCOPY (HR-DOSY) - A NEW TOOL FOR THE ANALYSIS OF COMPLEX-MIXTURES [J].
BARJAT, H ;
MORRIS, GA ;
SMART, S ;
SWANSON, AG ;
WILLIAMS, SCR .
JOURNAL OF MAGNETIC RESONANCE SERIES B, 1995, 108 (02) :170-172
[6]   High-performance liquid chromatography with nuclear magnetic resonance detection applied to organosilicon polymers -: Part 2:: Comparison with other methods [J].
Blechta, Vratislav ;
Kurfurst, Milan ;
Sykora, Jan ;
Schraml, Jan .
JOURNAL OF CHROMATOGRAPHY A, 2007, 1145 (1-2) :175-182
[7]   J-modulation effects in DOSY experiments and their suppression: The Oneshot45 experiment [J].
Botana, Adolfo ;
Aguilar, Juan A. ;
Nilsson, Mathias ;
Morris, Gareth A. .
JOURNAL OF MAGNETIC RESONANCE, 2011, 208 (02) :270-278
[8]   Improving the accuracy of pulsed field gradient NMR diffusion experiments: Correction for gradient non-uniformity [J].
Connell, Mark A. ;
Bowyer, Paul J. ;
Bone, P. Adam ;
Davis, Adrian L. ;
Swanson, Alistair G. ;
Nilsson, Mathias ;
Morris, Gareth A. .
JOURNAL OF MAGNETIC RESONANCE, 2009, 198 (01) :121-131
[9]   13C PGSE NMR experiment with heteronuclear dipolar decoupling to measure diffusion in liquid crystals and solids [J].
Dvinskikh, SV ;
Sitnikov, R ;
Furó, I .
JOURNAL OF MAGNETIC RESONANCE, 2000, 142 (01) :102-110
[10]   Isomer Resolution by Micelle-Assisted Diffusion-Ordered Spectroscopy [J].
Evans, Robert ;
Haiber, Stephan ;
Nilsson, Mathias ;
Morris, Gareth A. .
ANALYTICAL CHEMISTRY, 2009, 81 (11) :4548-4550