Contact Surface of Heme Proteins to Water Studied by NMR Method.

(1)对称结构核磁共振管：在磁场分布分析的基础上，设计并测试了对称结构核磁共振管。原型使用小容器作为垫片塞。处理的困难促使开发一种简化的版本，使用与水性样品的磁化率相匹配的特殊玻璃。经过多次试验，这种具有对称几何形状的简化NMR微池是成功的，现在可以商业化。(2)一种新颖的选择性激励方法：选择性激励脉冲法为数不少，每种方法都有其自身的缺点。新方法利用11脉冲法。与传统的11脉冲方法相反，该方法使用对称的11个脉冲，并采用从11个脉冲获得的2组光谱的线性组合。这种新的方法是免费的基线滚动和相位失真。而且，信号抑制比肯定优于1331脉冲法。(3)N ...更多信息 非选择性完全饱和法：X核的NMR测量利用质子的非选择性饱和。这些方法在考虑质子饱和度本身时是不完善的。通过同时施加渐进饱和脉冲和沃脉冲，获得完全非选择性饱和。剩余质子共振小于1%。(4)顺磁离子在水溶液中的新弛豫机制：当水溶液中存在少量顺磁离子时，当H_2O信号的核自旋饱和时，顺磁离子的电子自旋很可能受到扰动。这种现象迄今为止在液相中是未知的。(5)大分子表面残留物的选择性观察：在少量顺磁性物质存在下进行饱和恢复。该方法能够观察到来自顺磁性物质附近的蛋白质的非常独特的选择性信号。因此，观察到的信号必须来自蛋白质分子上的表面残基。这种方法原则上普遍适用于任何大分子。少

(1) NMR tubes with symmetric geometry: Based on the analyses of magnetic field distribution, NMR tubes with symmetric geometry was devised and tested. Prototype used small containers for the purpose of shim plugs. Difficulty in handling prompted to develop a simplified version using a special glass matched with the magnetic susceptibility of aqueous samples. After several trials, this simplified NMR microcell with symmetric geometry was successful and now commercially available.(2) A novel selective excitation method: There are not a few selective excitation pulse method each of which has its own drawbacks. The novel method makes use of 11 pulse method. On the contrary to the conventional 11 pulse method, this method uses as symmetric 11 pulses and takes a linear combination of 2 sets of spectra obtained from 11 pulses. This new method is free from a baseline roll and phase distortions. Moreover, signal suppression ratio is certainly better than that obtained by 1331 pulse method.(3) N … More on-selective complete saturation method: NMR measurements of X nuclei make use of non-selective saturation of protons. These methods turns out imperfect concerning to proton saturation itself. By applying progressive saturation pulse and Waugh pulse simultaneously, complete non-selective saturation was obtained. Residual proton resonances were less than 1%.(4) New relaxation mechanism for paramagnetic ions in aqueous solution: When small amount of paramagnetic ions are present in a non-deuterated aqueous solution, and when nuclear spins of H_2O signal is saturated, it was found that electron spins of paramagnetic ions are most likely perturbed. This phenomenon has been unknown so far in a liquid phase.(5) Selective observation of surface residues on macromolecules: Saturation recovery was conducted under the presence of small amount of paramagnetic species. This method enabled to observe quite unique selective signals from proteins in the vicinity of paramagnetic species. Thus, the signals observed have to be derived from the surface residues on the protein molecules. This method is universally applicable to any macromolecules in principle. Less