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多重编辑HSQC中利用同步反转扫描补偿重聚焦效率低下(CRISIS)

Compensation of refocusing inefficiency with synchronized inversion sweep (CRISIS) in multiplicity-edited HSQC.

作者信息

Boyer Robert D, Johnson Ross, Krishnamurthy Krish

机构信息

Discovery Chemistry Research and Technologies, Lilly Research Laboratories, Indianapolis, IN 46285, USA.

出版信息

J Magn Reson. 2003 Dec;165(2):253-9. doi: 10.1016/j.jmr.2003.08.009.

Abstract

Use of adiabatic pulses in broadband inversion and decoupling is well known. Replacement of the rectangular pi pulses in the INEPT and rev-INEPT parts of the HSQC and gHSQC experiments with adiabatic pulses substantially improves the sensitivity of these experiments. However, modulation of cross peak intensity in multiplicity-edited HSQC or gHSQC experiments can be quite severe. These modulations arise during the multiplicity-editing periods due to the inefficient refocusing of the spin-echo caused by the mismatch of the echo delay with the one-bond coupling constant. These modulations (which we call echo modulations) are field strength (and hence spectral width) independent. Use of adiabatic pulses with the inversion sweep synchronized to the 1H-13C coupling constant range typically observed in a 13C spectrum will provide substantial improvement in sensitivity. The inversion profile problems associated with rectangular pi pulses can be moderately compensated by composite pulse schemes and these schemes could prove to be reasonable alternatives to adiabatic pulses. However, the adiabatic sweep provides a unique method to compensate the echo modulations for multiplicity-edited experiments. The origin and the compensation of refocusing inefficiency with synchronized inversion sweep (CRISIS) method to minimize these modulations is described.

摘要

在宽带反转和解耦中使用绝热脉冲是众所周知的。在HSQC和gHSQC实验的INEPT和rev-INEPT部分用绝热脉冲取代矩形π脉冲可显著提高这些实验的灵敏度。然而,在多重性编辑的HSQC或gHSQC实验中,交叉峰强度的调制可能相当严重。这些调制在多重性编辑期间出现,是由于回波延迟与一键耦合常数不匹配导致自旋回波的重聚焦效率低下。这些调制(我们称之为回波调制)与场强(以及光谱宽度)无关。使用反转扫描与通常在13C谱中观察到的1H-13C耦合常数范围同步的绝热脉冲将显著提高灵敏度。与矩形π脉冲相关的反转轮廓问题可以通过复合脉冲方案适度补偿,这些方案可能被证明是绝热脉冲的合理替代方案。然而,绝热扫描提供了一种独特的方法来补偿多重性编辑实验中的回波调制。本文描述了使用同步反转扫描(CRISIS)方法最小化这些调制的重聚焦效率低下的起源和补偿方法。

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