GLYCOSYL COMPOSITION ANALYSIS OF PORCINE INTESTINAL HEPARINS

在瓦里安Inova 600-MHz上进行了~1H-核磁共振分析 分光计。样品用冷冻干燥的方法进行了换氢处理。 从D2O中提取，并溶解在0.5mLDMSO-D6/D2O 982中。一维1H-核磁共振 利用预饱和在308(K(35(C))在600 MHz下获得光谱 残留的HOD信号。化学位移的测量相对于 2.503 ppm的剩余质子化二甲基亚砜-d6(间接测量 相对于TMS=0.0ppm)。正离子模式FAB质谱图是 使用JEOL SX/SX102A串联的前两个扇区获得 四扇区质谱计的加速电位为 10千伏。采用线性向上扫描，使得质量范围 从m/z 100到2500的扫描在1分钟内完成。两者的应用 技术确认了神经节苷脂的身份 多聚糖的结构、分子量分布和 目前存在的神经酰胺类型，以及总体纯度。

1H-NMR analysis was performed on a Varian Inova 600-MHz spectrometer. The sample was deuterium-exchanged by lyophilization from D2O and dissolved in 0.5 mL DMSO-d6/D2O 982. The 1D 1H-NMR spectrum was obtained at 308(K (35(C) at 600 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 spectrum was 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 identity of the ganglioside with respect to the structure of the glycan, the molecular weight distribution and type of ceramides present, and the overall purity.