FAB MS & NMR ANALYSIS OF GANGLIOSIDE

FAB质谱

• 批准号: 6653582
• 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/6653582
• 关键词: biological products; biomedical resource; carbohydrates; lipids; nuclear magnetic resonance spectroscopy; spectrometry

1H-NMR analyses were performed on a Bruker AMX-500 spectrometer. The samples were deuterium-exchanged by lyophilization from D2O and dissolved in 0.5 mL DMSO-d6/D2O 982. The 1D 1H-NMR spectra were obtained at 308(K (35(C) at 500 MHz, using presaturation of the residual HOD signal. Chemical shifts were measured relative to the residual protonated DMSO-d6 at 2.503 ppm (measured indirectly relative to TMS=0.0ppm). The positive ion mode FAB mass spectra were obtained using the first two sectors of a JEOL SX/SX102A tandem four-sector mass spectrometer operated at an acceleration potential of 10 kV. Linear upward scanning was employed such that the mass range from m/z 100 to 2500 is scanned in 1 minute. Application of both techniques confirmed the identities of two of the gangliosides with respect to their glycan structures, the molecular weight distribution and type of ceramides present, and their overall purity. The third ganglioside sample was found to be a very im pure preparation, as indicated by both NMR and FAB-MS analysis.

在Bruker AMX-500光谱仪上进行1H-NMR分析。 样品通过从D2 O冻干进行氘交换， 溶于0.5 mL DMSO-d 6/D2 O 982中。 1D 1H-NMR谱为： 在308（K）（35（C），500 MHz下，使用预饱和的 剩余HOD信号。 测量相对于化合物的化学位移。 2.503 ppm处的残留质子化DMSO-d 6（间接相对测量 至TMS=0.0ppm）。 获得了正离子模式FAB质谱 使用JEOL SX/SX 102 A串联四扇区的前两个扇区 质谱仪在10 kV的加速电位下操作。 采用线性向上扫描，使得质量范围从m/z 1分钟内扫描100到2500个。 两种技术的应用 确认了两种神经节苷脂的身份， 它们的聚糖结构、分子量分布和 存在的神经酰胺和它们的总纯度。 第三类神经节苷脂 发现样品是非常不纯的制备物，如由 NMR和FAB-MS分析。