NMR ANALYSIS OF AN OLIGOSACCHARIDE

低聚糖的 NMR 分析

• 批准号: 6653579
• 负责人: STEVEN B LEVERY
• 金额: $ 28.8万
• 依托单位: UNIVERSITY OF GEORGIA
• 依托单位国家: 美国
• 财政年份: 2002
• 资助国家: 美国
• 起止时间: 2002-08-01 至 2003-07-31
• 项目状态: 已结题
• 来源: https://reporter.nih.gov/project-details/6653579
• 关键词: biological products; biomedical resource; carbohydrates; nuclear magnetic resonance spectroscopy; technology /technique

1H-NMR analysis was performed on a Varian Inova 600-MHz spectrometer. The sample was deuterium-exchanged by lyophilization from D2O (2 X by sonication for a half hour, and lyophilization), and then dissolved in 0.7 mL D2O for NMR analysis (sonication for a half hour, followed by centrifugation at 3500 rpm for a half hour and transfer of the supernatant to the NMR tube). Since this procedure left considerable insoluble material, the process of sonication in D2O, centrifugation, and transfer was repeated to produce a second sample for comparison with the first. 1H-NMR 1-D and 2-D TOCSY (total correlation spectroscopy), and NOESY (nuclear Overhauser effect spectroscopy) experiments, as well as 1H-detected 1H-13C-gHSQC (gradient heteronuclear single quantum correlation) and -gHMBC (gradient heteronuclear multiple-bond correlation) experiments were performed at 25(C on the first sample. Proton and carbon chemical shifts were measured relative to internal acetone standard s ((=2.225 ppm and 29.9 ppm, respectively). A 1H-NMR 1-D spectrum of the second sample was obtained purely for comparison of spectral features and peak integration. Complete 1H- and 13C-resonance assignments were obtained by TOCSY and HSQC experiments, and the average repeating structure elucidated from interpretation of the HMBC and NOESY experiments.

在Varian Inova 600-MHz上进行1H-NMR分析。 光谱仪 样品通过冻干进行氘交换 从D2 O（2 X，超声处理半小时，冻干），和 然后溶解于0.7 mL D2 O中进行NMR分析（超声处理一半 小时，然后以3500 rpm离心半小时， 将上清液转移到NMR管中）。 由于这一程序 留下相当多的不溶性物质，超声处理的过程中， 重复D2 O、离心和转移，以产生第二个 与第一个样本进行比较。 1H-NMR一维和二维TOCSY（总 相关光谱）和NOESY（核Overhauser效应 光谱）实验，以及1H-检测的1H-13 C-gHSQC （梯度异质结单量子相关）和-gHMBC （梯度异质多重键相关）实验， 在25 ℃下对第一个样品进行。 质子和碳化学 相对于内标丙酮S（=2.225 ppm和29.9ppm）。 第二个化合物的1H-NMR 1-D光谱 获得样品纯粹是为了比较光谱特征， 峰值积分 完整的1H-和13 C-共振分配如下： 通过TOCSY和HSQC实验获得， 根据HMBC和NOESY的解释阐明的结构 实验