Quantitative two-dimensional HSQC experiment for high magnetic field NMR spectrometers

被引:48
|
作者
Koskela, Harri [1 ]
Heikkila, Outi [2 ]
Kilpelainen, Ilkka [3 ]
Heikkinen, Sami [3 ]
机构
[1] Univ Helsinki, VERIFIN, FIN-00014 Helsinki, Finland
[2] Univ Helsinki, Folkhalsan Inst Genet, Folkhalsan Res Ctr, FIN-00014 Helsinki, Finland
[3] Univ Helsinki, Organ Chem Lab, FIN-00014 Helsinki, Finland
关键词
Quantitative two-dimensional NMR; (13)C offset compensation; Carr-Purcell-Meiboom-Gill sequence; Adiabatic inversion pulses; PM-BEBOP; Q-OCCAHSQC; Human blood plasma; BROAD-BAND INVERSION; MULTIPLICITY-EDITED HSQC; HUMAN BLOOD-PLASMA; ADIABATIC PULSES; H-1-NMR SPECTROSCOPY; COMPOSITE PULSES; POLARIZATION TRANSFER; POPULATION-INVERSION; REFOCUSING PULSES; SINGLE-SCAN;
D O I
10.1016/j.jmr.2009.09.021
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
The finite RF power available on carbon channel in proton-carbon correlation experiments leads to non-uniform cross peak intensity response across carbon chemical shift range. Several classes of broadband pulses are available that alleviate this problem. Adiabatic pulses provide an excellent magnetization inversion over a large bandwidth, and very recently, novel phase-modulated pulses have been proposed that perform 900 and 1800 magnetization rotations with good offset tolerance. Here, we present a study how these broadband Pulses (adiabatic and phase-modulated) can improve quantitative application of the heteromolecular single quantum coherence (HSQC) experiment on high magnetic field strength NMR spectrometers. Theoretical and experimental examinations of the quantitative, offset-compensated. CPMG-adjusted HSQC (Q-OCCAHSQC) experiment are presented. The proposed experiment offers a formidable improvement to the offset performance; (13)C offset-dependent standard deviation of the peak intensity was below 6% in range of +/- 20 kHz. This covers the carbon chemical shift range of 150 ppm, which contains the protonated carbons excluding the aldehydes, for 22.3 T NMR magnets. A demonstration of the quantitative analysis of a fasting blood plasma sample obtained from a healthy volunteer is given. (C) 2009 Elsevier Inc. All rights reserved.
引用
收藏
页码:24 / 33
页数:10
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