GLYCOSYL COMPOSITION ANALYSIS OF PORCINE INTESTINAL HEPARINS

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 将反应混合物从D2 O中除去，并溶解于0.5 mL DMSO-d 6/D2 O 982中。 一维1H-NMR 使用预饱和法在308 K（35 ℃）和600 MHz下获得光谱 剩余的HOD信号。 测量化学位移相对于 残留的质子化DMSO-d 6为2.503 ppm（间接测量 相对于TMS=0.0ppm）。 正离子模式FAB质谱为 使用JEOL SX/SX 102 A串联的前两个扇区获得 四扇区质谱仪在加速电位下运行， 10千伏。 采用线性向上扫描，使得质量范围 从m/z 100到2500在1分钟内扫描。 应用两 技术证实了神经节苷脂的身份， 聚糖的结构、分子量分布和 存在的神经酰胺的类型和总纯度。

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.