NMR ANALYSIS OF OLIGOSACCHARIDES

通过以下方法分析样品的单糖组成： 制备甲基糖苷的三甲基硅基衍生物， 然后进行气相色谱（GC）和合并的气体 色谱/质谱（GC-MS）分析。 TMS 通过在3 M甲醇中甲醇分解从样品制备甲基糖苷 HCl，氨基糖与吡啶和乙酸的再-N-乙酰化 在甲醇中的酸酐，和用Tri-Sil的全-O-三甲基甲硅烷基化。 GC TMS甲基糖苷的分析在HP 5890 GC上进行 使用DB 1熔融石英毛细管柱。 GC-MS分析 使用与5970 MSD连接的HP 5890 GC进行。 单糖通过它们的保留时间进行鉴定， 标准，这些碳水化合物的特征是 通过它们的质谱进行鉴定

The samples were analyzed for monosaccharide composition by preparing the trimethylsilyl derivatives of the methylglycosides followed by gas chromatography (GC) and combined gas chromatography/mass spectrometry (GC-MS) analysis. TMS methylglycosides were prepared from the sample by methanolysis in 3 M HCl, re-N-acetylation of amino sugars with pyridine and acetic anhydride in methanol, and per-O-trimethylsilylation with Tri-Sil. GC analysis of the TMS methylglycosides was performed on an HP5890 GC using a DB1 fused silica capillary column. GC-MS analysis was performed using an HP 5890 GC interfaced to a 5970 MSD. Monosaccharides were identified by their retention times in comparison to standards, and the carbohydrate character of these was authenticated by their mass spectra.