Magnetization transfer magic-angle-spinning z-spectroscopy of excised tissues

Magnetization transfer magic-angle-spinning z-spectroscopy of excised tissues
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DOI:
10.1016/j.jmr.2009.03.007
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发表时间:
2009-07-01
影响因子:
2.2
通讯作者:
Frydman, Ludo
Frydman, Ludo
中科院分区:
化学3区
文献类型:
--
作者:
Avni, Reut;Mangoubi, Oren;Frydman, Ludo

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设计用于组织分析的核磁共振实验包括磁化转移(MT)和高分辨率魔角自旋(HRMAS)方法,磁化转移(MT)可以通过交叉弛豫和/或体H-1水共振的化学交换过程来突出生物大分子的信号,高分辨率魔角自旋(HRMAS)方法类似于固态核磁共振中使用的方法,通过自旋各向异性的平均来引入额外的光谱分辨率。本文探讨了结合这些方法的结果,并报道了在各种HRMAS条件下切除组织中水和细胞成分之间的MT“z-光谱”。从H-1“MTMAS”实验中得到的主要特征包括以液液水位移为中心的强自旋边带流形,与脂肪族和酰胺质子共振一致的高分辨率各向同性特征,以及随着自旋速度的增加而出现的第二边带流形。对这些不同特征的起源进行了解释,包括模拟,进一步阐明了对组织样品观察到的MT核磁共振信号的性质。同时,组织学检查报告验证了HRMAS核磁共振程序的局限性,以许多不同的方式保存的组织样本的分析。(C) 2009爱思唯尔公司版权所有。
NMR experiments devised to aid in analyses Of tissues include magnetization transfer (MT), which can highlight the signals of biological macromolecules through cross-relaxation and/or chemical exchange processes with the bulk H-1 water resonance, and high-resolution magic-angle-spinning (HRMAS) methods, akin to those used in solid-state NMR to introduce additional spectral resolution via the averaging of spin anisotropies. This paper explores the result of combining these methodologies, and reports on MT "z-spectroscopy" between water and cell components in excised tissues under a variety of HRMAS conditions. Main features arising from the resulting H-1 "MTMAS" experiments include strong spinning sideband manifolds centered at the liquid water shift, high-resolution isotropic features coinciding with aliphatic and amide proton resonances, and a second sideband manifold arising as spinning speeds are increased. Interpretations are given for the origin of these various features, including simulations shedding further light onto the nature of MT NMR signals observed for tissue samples. Concurrently, histological examinations are reported validating the limits of HRMAS NMR procedures to the analysis of tissue samples preserved in a number of different ways. (C) 2009 Elsevier Inc. All rights reserved.