溶液中高场和低场核磁共振光谱的稳态自由进动序列:挑战和机遇

Tiago Bueno Moraes , Flávio Vinícius Crizóstomo Kock , Kahlil Schwanka Salome , Andersson Barison , Andre Simpson , Luiz Alberto Colnago
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引用次数: 1

摘要

与其他技术相比,核磁共振光谱的接受度较低。历史上,增加静态磁场的强度一直是提高核磁共振灵敏度的主要方法。近年来,一些极化传输协议已被用于提高信噪比(SNR),尽管它们需要特殊的附件和/或样品制备。在本文中,我们考虑了稳态自由进动(SSFP)脉冲序列作为提高标准高分辨率和台式低分辨率核磁共振光谱仪信噪比的一种简单有效的替代方法所面临的挑战和机遇。在这些序列中,以最短的脉冲间隔时间(Tp)获得最大增益。然而,当Tp<T2时,SSFP信号包含FID和回波分量,导致快速傅里叶变换(FT)得到的光谱存在相位、强度和截断伪影。采用了几个相位交替的SSFP序列来抵消回波分量,从而最大限度地减少了FT谱中的这些问题。Krylov碱基对角化方法(KBDM)用于消除SSFP脉冲序列获得的光谱中的相位和截断问题,可以作为FT的可行替代方法。实验在高分辨率和低分辨率(bench - top)核磁共振光谱仪上进行,可以显著提高低接受度核(如13C和15N)的信噪比。在非常稀的样品中,SSFP序列也被证明可以提高19F和31P等高接受性核的信噪比,这在环境和生物样品中很常见。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

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Steady-State Free Precession sequences for high and low field NMR spectroscopy in solution: Challenges and opportunities

The receptivity of NMR spectroscopy is low when compared to other techniques. Historically, increasing the strength of the static magnetic field has been the major approach to increase NMR sensitivity. In recent years several polarization transfer protocols have been used to enhance the signal-to-noise ratio (SNR), although they require special accessories and/or sample preparation. In this paper, we consider both the challenges and opportunities of steady-state free precession (SSFP) pulse sequences as a simple and efficient alternative to enhance SNR, in standard high-resolution and benchtop low-resolution NMR spectrometers. The maximum gain in these sequences is obtained with the shortest time between the pulses (Tp). However, when Tp<T2, the SSFP signal contains FID and echo components which lead to phase, intensity, and truncation artifacts on spectra obtained by Fast Fourier transform (FT). Several phase alternation SSFP sequences were used to cancel the echo component and minimize these problems in the FT spectra. Krylov base diagonalization method (KBDM) was used to eliminate the phase and truncation problems in spectra acquired by SSFP pulse sequences and can be a viable alternative to FT. The experiments were performed in high and low resolution (bench top) NMR spectrometers and significant enhancements in SNR of low receptivity nuclei such as 13C and 15N could be achieved. The SSFP sequences were also shown to enhance SNR in nuclei with high receptivity such as 19F and 31P, in very dilute samples, as is common in environmental and biological samples.

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