Longitudinal 1H relaxation optimization in TROSY NMR spectroscopy
Longitudinal 1H relaxation optimization in TROSY NMR spectroscopy
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DOI：
10.1021/ja027149q
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发表时间：
2002-10-30
影响因子：
15
通讯作者：
Eletsky, A
中科院分区：
文献类型：
--
作者：
Pervushin, K;Vögeli, B;Eletsky, A
本文描述了一种通过显著减少质子纵向弛豫时间来提高在高极化磁场下进行的多维核磁共振实验灵敏度的一般方法。该方法是基于在C-13、N-15标记和完全质子化或部分氘化的蛋白质中使用两个巨大的“热浴”H-1自旋，这些自旋位于共价连接碳和氧原子的氢上，以均匀地增强H-1(N)自旋的纵向弛豫，并同时提高多脉冲核磁共振实验的灵敏度。在二维[N-15，H-1]-LTROSY、二维[N-15，H-1]-LHSQC和三维LTROSY-HNCA实验中实现了所提出的纵向松弛优化，在600 MHz下单位时间最大信噪比提高了2-2.5倍。在900 MHz时，预测的(HN)-H-1纵向弛豫时间的减少可达一个数量级，使该方法成为高磁场下蛋白质核磁共振的重要工具。
A general method to enhance the sensitivity of the multidimensional NMR experiments performed at high-polarizing magnetic field via the significant reduction of the longitudinal proton relaxation times is described. The method is based on the use of two vast pools of "thermal bath" H-1 spins residing on hydrogens covalently attached to carbon and oxygen atoms in C-13,N-15 labeled and fully protonated or fractionally deuterated proteins to uniformly enhance longitudinal relaxation of the H-1(N) spins and concomitantly the sensitivity of multipulse NMR experiments. The proposed longitudinal relaxation optimization is implemented in the 2D [N-15,H-1]-LTROSY, 2D [N-15,H-1]-LHSQC and 3D LTROSY-HNCA experiments yielding the factor 2-2.5 increase of the maximal signal-to-noise ratio per unit time at 600 MHz. At 900 MHz, the predicted decrease of the (HN)-H-1 longitudinal relaxation times can be as large as one order of magnitude, making the proposed method an important tool for protein NMR at high magnetic fields.