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.

1H-NMR分析在Varian Inova 600-MHz上进行 光谱仪。 样品是通过冻干的氘化处理的 从D2O（通过超声处理2 x，半小时，冻干），然后 然后溶解在0.7 mL D2O中进行NMR分析（一半超声处理 小时，然后在3500 rpm的3500 rpm离心半小时，然后 将上清液转移到NMR管）。 由于此过程 留下相当大的不溶性材料，超声处理的过程 重复D2O，离心和转移以产生第二个 样品以与第一个进行比较。 1H-NMR 1-D和2-D TOCSY（总计 相关光谱法）和贵族（核透射效应 光谱）实验以及1H检测的1H-13C-GHSQC （梯度异核单量子相关）和-GHMBC （梯度异核多键相关）实验是 在第25个（第一个样品上进行C。Proton和Carbon Chemical）进行 相对于内部丙酮标准s测量移位（（（= 2.225） ppm和29.9 ppm）。 第二秒的1H-NMR 1-D光谱 纯粹获得样品以比较光谱特征和 峰积分。 完成的1H和13C共振分配是 由Tocsy和HSQC实验获得，平均重复 从HMBC和Noesy的解释中阐明的结构 实验。