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在高 MAS 频率下采用低功率基于对称的混合方案的化学位移相关。

Chemical shift correlation at high MAS frequencies employing low-power symmetry-based mixing schemes.

机构信息

Department of Physics, Ubon Ratchathani University, Thailand.

出版信息

J Biomol NMR. 2011 Jul;50(3):277-84. doi: 10.1007/s10858-011-9516-2. Epub 2011 Jun 11.

DOI:10.1007/s10858-011-9516-2
PMID:21674236
Abstract

An approach for conveniently implementing low-power CN ( n ) (ν) and RN ( n ) (ν) symmetry-based band-selective mixing sequences for generating homo- and heteronuclear chemical shift correlation NMR spectra of low γ nuclei in biological solids is demonstrated. Efficient magnetisation transfer characteristics are achieved by selecting appropriate symmetries requiring the application of basic RF elements of relatively long duration and numerically tailoring the RF field modulation profile of the basic element. The efficacy of the approach is experimentally shown by the acquisition of (15)N-(13)C dipolar and (13)C-(13)C scalar and dipolar coupling mediated chemical shift correlation spectra at representative MAS frequencies.

摘要

本文展示了一种方便实现低功率 CN(n)(ν)和 RN(n)(ν)对称基带选择混合序列的方法,用于生成生物固体中低γ核的同核和异核化学位移相关 NMR 谱。通过选择适当的对称性,可以实现有效的磁化转移特性,这些对称性要求应用相对较长持续时间的基本 RF 元件,并对基本元件的 RF 场调制轮廓进行数值调整。通过在代表性的 MAS 频率下采集 (15)N-(13)C 偶极和 (13)C-(13)C 标量和偶极耦合介导的化学位移相关谱,实验证明了该方法的有效性。

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本文引用的文献

1
Broadband 15N-13C dipolar recoupling via symmetry-based RF pulse schemes at high MAS frequencies.基于对称射频脉冲方案在高 MAS 频率下实现宽带 15N-13C 双共振去耦。
J Biomol NMR. 2010 May;47(1):7-17. doi: 10.1007/s10858-010-9406-z. Epub 2010 Mar 20.
2
Symmetry-based dipolar recoupling by optimal control: band-selective experiments for assignment of solid-state NMR spectra of proteins.基于对称的最优控制偶极重耦合:用于蛋白质固态核磁共振谱归属的带选择性实验
J Chem Phys. 2009 Jul 14;131(2):025101. doi: 10.1063/1.3157737.
3
Numerical design of RN(n)(nu) symmetry-based RF pulse schemes for recoupling and decoupling of nuclear spin interactions at high MAS frequencies.
异步通过键同核各向同性混合:在魔角旋转下应用于全氘代蛋白质中的碳-碳转移
J Biomol NMR. 2015 Nov;63(3):245-53. doi: 10.1007/s10858-015-9980-1. Epub 2015 Aug 30.
4
MAS solid state NMR of proteins: simultaneous ¹⁵N- ¹³CA and ¹⁵N- ¹³CO dipolar recoupling via low-power symmetry-based RF pulse schemes.蛋白质的MAS固态核磁共振:通过基于低功率对称性的射频脉冲序列实现¹⁵N-¹³CA和¹⁵N-¹³CO双极耦合同时进行
J Biomol NMR. 2015 May;62(1):7-15. doi: 10.1007/s10858-015-9910-2. Epub 2015 Feb 25.
5
Solid state NMR of proteins at high MAS frequencies: symmetry-based mixing and simultaneous acquisition of chemical shift correlation spectra.高 MAS 频率下的蛋白质固态 NMR:基于对称性的混合和化学位移相关谱的同时采集。
J Biomol NMR. 2012 Dec;54(4):325-35. doi: 10.1007/s10858-012-9680-z. Epub 2012 Nov 23.
6
Dual-band selective double cross polarization for heteronuclear polarization transfer between dilute spins in solid-state MAS NMR.固态 MAS NMR 中稀核之间异核极化转移的双频选择双交叉偏振。
J Magn Reson. 2012 Apr;217:92-9. doi: 10.1016/j.jmr.2012.02.020. Epub 2012 Mar 5.
基于RN(n)(nu)对称性的射频脉冲序列的数值设计,用于在高魔角旋转频率下实现核自旋相互作用的再耦合和解耦
J Biomol NMR. 2009 Aug;44(4):235-44. doi: 10.1007/s10858-009-9335-x. Epub 2009 Jun 26.
4
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J Biomol NMR. 2009 Aug;44(4):175-84. doi: 10.1007/s10858-009-9334-y. Epub 2009 Jun 23.
5
Design of high-power, broadband 180 degrees pulses and mixing sequences for fast MAS solid state chemical shift correlation NMR spectroscopy.用于快速MAS固态化学位移相关核磁共振光谱的高功率宽带180度脉冲和混合序列设计。
J Biomol NMR. 2009 Jan;43(1):51-61. doi: 10.1007/s10858-008-9292-9. Epub 2008 Nov 19.
6
J-based 2D homonuclear and heteronuclear correlation in solid-state proteins.基于 J 的固态蛋白质的二维同核和异核相关。
Magn Reson Chem. 2007 Dec;45 Suppl 1:S84-92. doi: 10.1002/mrc.2107.
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Solid-state protein-structure determination with proton-detected triple-resonance 3D magic-angle-spinning NMR spectroscopy.利用质子检测的三重共振三维魔角旋转核磁共振光谱法进行固态蛋白质结构测定。
Angew Chem Int Ed Engl. 2007;46(44):8380-3. doi: 10.1002/anie.200702905.
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Proton-detected solid-state NMR spectroscopy of fully protonated proteins at 40 kHz magic-angle spinning.在40千赫兹魔角旋转条件下对完全质子化蛋白质进行质子检测的固态核磁共振光谱学。
J Am Chem Soc. 2007 Sep 26;129(38):11791-801. doi: 10.1021/ja073462m. Epub 2007 Aug 29.
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Backbone assignments in solid-state proteins using J-based 3D heteronuclear correlation spectroscopy.使用基于J的三维异核相关光谱法进行固态蛋白质的主链归属
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10
Optimal control based NCO and NCA experiments for spectral assignment in biological solid-state NMR spectroscopy.基于最优控制的生物固态核磁共振光谱中谱峰归属的NCO和NCA实验
J Magn Reson. 2007 Oct;188(2):216-30. doi: 10.1016/j.jmr.2007.06.011. Epub 2007 Jul 7.