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在魔角旋转下进行高分辨率检测的场循环核磁共振:光合反应中心中核超极化场窗口的测定

Field-cycling NMR with high-resolution detection under magic-angle spinning: determination of field-window for nuclear hyperpolarization in a photosynthetic reaction center.

作者信息

Gräsing Daniel, Bielytskyi Pavlo, Céspedes-Camacho Isaac F, Alia A, Marquardsen Thorsten, Engelke Frank, Matysik Jörg

机构信息

Institut für Analytische Chemie, Universität Leipzig, Linnéstraße 3, D-04103, Leipzig, Germany.

Escuela de Química, Tecnológico de Costa Rica, Sede Central, 30101, Cartago, Costa Rica.

出版信息

Sci Rep. 2017 Sep 21;7(1):12111. doi: 10.1038/s41598-017-10413-y.

Abstract

Several parameters in NMR depend on the magnetic field strength. Field-cycling NMR is an elegant way to explore the field dependence of these properties. The technique is well developed for solution state and in relaxometry. Here, a shuttle system with magic-angle spinning (MAS) detection is presented to allow for field-dependent studies on solids. The function of this system is demonstrated by exploring the magnetic field dependence of the solid-state photochemically induced nuclear polarization (photo-CIDNP) effect. The effect allows for strong nuclear spin-hyperpolarization in light-induced spin-correlated radical pairs (SCRPs) under solid-state conditions. To this end, C MAS NMR is applied to a photosynthetic reaction center (RC) of the purple bacterium Rhodobacter (R.) sphaeroides wildtype (WT). For induction of the effect in the stray field of the magnet and its subsequent observation at 9.4 T under MAS NMR conditions, the sample is shuttled by the use of an aerodynamically driven sample transfer technique. In the RC, we observe the effect down to 0.25 T allowing to determine the window for the occurrence of the effect to be between about 0.2 and 20 T.

摘要

核磁共振(NMR)中的几个参数取决于磁场强度。场循环核磁共振是探索这些性质的场依赖性的一种巧妙方法。该技术在溶液状态和弛豫测量方面已得到充分发展。在此,提出了一种具有魔角旋转(MAS)检测的穿梭系统,以进行对固体的场依赖性研究。通过探索固态光化学诱导核极化(光-CIDNP)效应的磁场依赖性来证明该系统的功能。该效应允许在固态条件下在光诱导的自旋相关自由基对(SCRPs)中实现强核自旋超极化。为此,将碳-13(C) MAS NMR应用于紫色细菌球形红杆菌(R.)野生型(WT)的光合反应中心(RC)。为了在磁体的杂散场中诱导该效应并随后在MAS NMR条件下于9.4 T下对其进行观察,使用空气动力学驱动的样品转移技术使样品穿梭移动。在RC中,我们观察到该效应低至0.25 T,从而能够确定该效应发生的窗口在约0.2至20 T之间。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/4666/5608766/76e02e82d4e5/41598_2017_10413_Fig1_HTML.jpg

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