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PITANSEMA-MAS,一种在魔角旋转(MAS)条件下测量异核偶极耦合的固态核磁共振方法。

PITANSEMA-MAS, a solid-state NMR method to measure heteronuclear dipolar couplings under MAS.

作者信息

Yamamoto K, Ermakov V L, Lee D K, Ramamoorthy A

机构信息

Biophysics Research Division and Department of Chemistry, University of Michigan, Ann Arbor, MI 48109-1055, United States.

出版信息

Chem Phys Lett. 2005 Jun 7;408(1-3):118-122. doi: 10.1016/j.cplett.2005.04.017.

DOI:10.1016/j.cplett.2005.04.017
PMID:16652173
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC1451416/
Abstract

A 2D NMR method is presented for the measurement of the dipole-dipole interaction between a proton and a low-frequency nuclear spin species in the solid state under the magic angle spinning. It employs the time averaged nutation concept to dramatically reduce the required radio frequency (rf) power on the low γ nuclear channel and spin exchange at the magic angle is used to suppress (1)H-(1)H dipolar interactions and chemical shifts. The flexibility in choosing the spinning speed, rf power and the scaling factor of the pulse sequence are of considerable importance for the structural studies of biological solids. The performance of the pulse sequence has been numerically and experimentally demonstrated on several solids.

摘要

本文提出了一种二维核磁共振方法,用于在魔角旋转条件下测量固态中质子与低频核自旋物种之间的偶极-偶极相互作用。该方法采用时间平均章动概念,显著降低了低γ核通道所需的射频功率,并利用魔角处的自旋交换来抑制(1)H-(1)H偶极相互作用和化学位移。选择旋转速度、射频功率和脉冲序列的缩放因子的灵活性对于生物固体的结构研究具有相当重要的意义。该脉冲序列的性能已在几种固体上进行了数值和实验验证。

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本文引用的文献

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Heteronuclear dipolar recoupling in solid-state nuclear magnetic resonance by amplitude-, phase-, and frequency-modulated Lee-Goldburg cross-polarization.通过幅度、相位和频率调制的李-戈德堡交叉极化实现固态核磁共振中的异核偶极重耦合。
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Heteronuclear polarization transfer by symmetry-based recoupling sequences in solid-state NMR.固态核磁共振中基于对称性的重耦合序列实现的异核极化转移
Solid State Nucl Magn Reson. 2004 Sep;26(2):57-64. doi: 10.1016/j.ssnmr.2003.11.001.
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Heteronuclear dipolar recoupling in liquid crystals and solids by PISEMA-type pulse sequences.通过PISEMA型脉冲序列实现液晶和固体中的异核偶极重耦合。
J Magn Reson. 2003 Sep;164(1):165-70. doi: 10.1016/s1090-7807(03)00180-0.
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Chemical shift anisotropy and offset effects in cross polarization solid-state NMR spectroscopy.交叉极化固态核磁共振光谱中的化学位移各向异性和偏移效应。
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An experimental strategy to dramatically reduce the RF power used in cross polarization solid-state NMR spectroscopy.一种显著降低交叉极化固态核磁共振光谱中所用射频功率的实验策略。
J Am Chem Soc. 2001 Aug 1;123(30):7467-8. doi: 10.1021/ja016212t.
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SIMPSON: a general simulation program for solid-state NMR spectroscopy.辛普森:一种用于固态核磁共振光谱学的通用模拟程序。
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Spin dynamics of polarization inversion spin exchange at the magic angle in multiple spin systems.多自旋系统中魔角处极化反转自旋交换的自旋动力学
J Magn Reson. 2000 Mar;143(1):136-43. doi: 10.1006/jmre.1999.1971.
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Recoupled polarization transfer heteronuclear 1H-13C multiple-quantum correlation in solids under ultra-fast MAS.超快磁共振条件下固体中再耦合极化转移异核1H-13C多量子相关
J Magn Reson. 1999 Oct;140(2):471-6. doi: 10.1006/jmre.1999.1856.
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Experimental aspects of multidimensional solid-state NMR correlation spectroscopy.多维固态核磁共振相关光谱学的实验方面
J Magn Reson. 1999 Sep;140(1):131-40. doi: 10.1006/jmre.1999.1827.
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13C-1H dipolar recoupling under very fast magic-angle spinning using virtual pulses.利用虚拟脉冲在极快速魔角旋转下实现的13C-1H偶极重新耦合
Solid State Nucl Magn Reson. 1999 May;13(4):203-12. doi: 10.1016/s0926-2040(99)00005-3.