4.3 Article

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

Journal

JOURNAL OF MAGNETIC RESONANCE
Volume 202, Issue 1, Pages 24-33

Publisher

ACADEMIC PRESS INC ELSEVIER SCIENCE
DOI: 10.1016/j.jmr.2009.09.021

Keywords

Quantitative two-dimensional NMR; (13)C offset compensation; Carr-Purcell-Meiboom-Gill sequence; Adiabatic inversion pulses; PM-BEBOP; Q-OCCAHSQC; Human blood plasma

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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.

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