Structural studies of alpha-bungarotoxin. 2. 1H NMR assignments via an improved relayed coherence transfer nuclear overhauser enhancement experiment.
Structural studies of alpha-bungarotoxin. 2. 1H NMR assignments via an improved relayed coherence transfer nuclear overhauser enhancement experiment.
复制标题
α-金环蛇毒素的结构研究。
DOI：
10.1021/bi00408a017
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发表时间：
1988
期刊：
影响因子：
2.9
通讯作者：
Scheek,RM
中科院分区：
文献类型：
--
作者：
Basus,VJ;Scheek,RM
材料与方法：样品制备。随后的论文（Kosen et al., 1988）描述了虫毒的纯化。这里使用的样品在95% H20-5% D20溶液中含有5-7毫米的虫毒，并以大约1毫米的丙酸钠（三甲基硅基）（TSP）作为化学位移参考。核磁共振光谱。所有光谱都是在上一篇论文（Basus et al., 1988）中描述的为HOHAHA实验而修改的通用电气gn -500核磁共振光谱仪上以800-1024 i[增量和时间比例相位增量程序（marion&w<e:1>, 1983）获得的。t2共获得4096个复杂数据点。零填充用于在t × t2维中分别创建1024 × 4096个数据点的最终实矩阵。在两个维度中都使用了6024 Hz的频谱宽度。将载流子频率置于H20共振上，除演化（fi）和采集（f2）周期外，所有时间都对其进行辐照。基线校正方法在之前的论文中描述过（Basus et al., 1988）。所有等高线图均以连续等高线水平之间的系数1.4绘制。
Materials and MethodsSample Preparation. Purificationof bungarotoxin is described in the succeeding paper (Kosen et al., 1988). Samples used here contained 5-7 mM bungarotoxin in 95% H20-5% D20 solution and with approximately 1 mM sodium (tri-methylsilyl) propionate (TSP) as a chemical shift reference. NMR Spectra. All spectra were obtained with 800-1024 i [increments and according to the time-proportional phase incrementation procedure (Marion& Wüthrich, 1983), on a General ElectricGN-500 NMR spectrometer modifiedfor the HOHAHA experiment as described in the previous paper (Basus et al., 1988). A total of 4096 complex data points were acquired in t2. Zero filling was used in tu creating a final real matrix of 1024 by 4096data points in the t¡ and t2 dimensions, respectively. Spectral widths of 6024 Hz were used in both dimensions. Thecarrier frequency was placed on the H20 resonance, which was irradiated at all times except for the evolution (fi) and acquisition (f2) periods. Base-line correction was used as described in the previous paper (Basus et al., 1988). All contour plots were plotted with a factor of 1.4 between consecutive contour levels.