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通过 H 检测和空间转移实现快速 MAS 下高分辨率四极矩/MQ/ST-HETCOR 2D 谱的快速采集。

Accelerating the acquisition of high-resolution quadrupolar MQ/ST-HETCOR 2D spectra under fast MAS via H detection and through-space population transfers.

机构信息

Bruker Japan K.K., 3-9, Moriya-cho, Kanagawa-ku, Yokohama-shi, Kanagawa 221-0022, Japan.

Univ. Lille, CNRS, INRAE, Centrale Lille, Univ. Artois, FR 2638 - IMEC - Institut Michel-Eugène Chevreul, F-59000 Lille, France.

出版信息

J Magn Reson. 2021 Dec;333:107093. doi: 10.1016/j.jmr.2021.107093. Epub 2021 Oct 21.

Abstract

Recently, we established an experimental setup protocol to perform the population transfer from half-integer quadrupolar spin to H nuclei under fast MAS in the context of MQ-HETCOR experiments. In this article, we further develop the high-resolution 2D HETCOR methods by ST-based approaches, making use of the sensitivity advantage of STMAS over its MQMAS counterpart. In a similar manner to the previous work, which utilized CP and RINEPT for the population transfer, we also demonstrate the experimental setup protocol for PRESTO. Using {Na}-H and {Al}-H spin systems of powder samples, we compare a series of MQ/ST-HETCOR 2D spectra to discuss the pros and cons of the distinct MQ/ST-based approaches for spin 3/2 and 5/2 nuclei, respectively. We also incorporate two experimental tricks to reduce the experimental time of such long 2D experiments, the Optimized Rotor-Synchronization (ORS) and the Non-Uniform Sampling (NUS), in the context of high-resolution spectra of half-integer quadrupolar spin nuclei.

摘要

最近,我们建立了一个实验设置方案,以在 MQ-HETCOR 实验的背景下,在快速 MAS 下将半整数四极自旋向 H 核进行种群转移。在本文中,我们通过基于 ST 的方法进一步发展了高分辨率的 2D HETCOR 方法,利用了 STMAS 相对于其 MQMAS 对应物的灵敏度优势。与之前利用 CP 和 RINEPT 进行种群转移的工作类似,我们还展示了 PRESTO 的实验设置方案。使用粉末样品的 {Na}-H 和 {Al}-H 自旋系统,我们比较了一系列 MQ/ST-HETCOR 2D 谱,以分别讨论不同的基于 MQ/ST 的方法对自旋 3/2 和 5/2 核的优缺点。我们还结合了两种实验技巧,即优化转子同步(ORS)和非均匀采样(NUS),以在半整数四极自旋核的高分辨率谱中减少这种长 2D 实验的实验时间。

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