GLYCOSYL COMPOSITION ANALYSIS OF LIPOPOLYSACCHARIDES FROM PREVOTELLA INTERMEDIA

通过对样品进行单糖组成分析 制备甲基葡萄糖苷的TMS衍生物 GC-MS分析。样品被酸解，然后进行 甲烷化后与吡啶和乙酸乙酯进行N-乙酰化反应 酸酐(用于检测氨基糖)。然后，样本被 用Tri-sil治疗。用气相色谱-质谱法分析了TMS中的甲基糖苷。 在HP5890 GC和5970 MSD上使用30米DB1执行 熔融石英毛细管柱。对这些样本进行了 用Hakomori甲基化程序进行糖基连锁分析 然后进行GC-MS联用分析。然后对样本进行了测试 用2M三氟乙酸酸进行酸解以实现切割 在所有的糖苷键中。糖基残基被还原为 NaBD4，然后用乙酸酐/吡啶进行乙酰化。这个 得到的部分甲基化的阿迪醇乙酸酯在 30米Supelco 2330熔融石英毛细管色谱柱 惠普5890 GC与5970 MSD配合使用。对样品进行了一维分析 在Bruker AMX-500型仪器上进行了~1H-NMR波谱分析。

The samples were analyzed for monosaccharide composition by preparing the TMS derivatives of the methylglycosides followed by GC-MS analysis. The samples were acid hydrolyzed then subjected to methanolysis followed by N-acetylation with pyridine and acetic anhydride (for detection of amino sugars). The samples were then treated with Tri-Sil. GC-MS analysis of the TMS methylglycosides was performed on an HP5890 GC coupled to a 5970 MSD using a 30-meter DB1 fused silica capillary column. The samples were subjected to glycosyl-linkage analysis using the Hakomori methylation procedure followed by combined GC-MS analysis. The samples were then subjected to acid hydrolysis using 2 M trifluoroacetic acid to effect cleavage of all glycosidic linkages. The glycosyl residues were reduced with NaBD4 and then acetylated using acetic anhydride/pyridine. The resulting partially methylated alditol acetates were analyzed on a 30-meter Supelco 2330 fused silica capillary column b y GC-MS using an HP 5890 GC coupled to a 5970 MSD. The samples were analyzed by 1-D 1H-NMRspectroscopy on a Bruker AMX-500 instrument.