植物组织中糖与糖醇乙酰化及毛细管气相色谱分析

介绍了一种用1-甲基咪唑为溶剂和催化剂、盐酸羟胺和乙酸酐为肟化和乙酰化试剂,对植物样品中糖与糖醇进行乙酰化衍生化后的气相色谱分离和质谱鉴定的分析方法.并对糖与糖醇乙酰化影响较大的反应温度、反应时间、反应物组成和反应物浓度等条件进行了比较研究,确定了糖与糖醇乙酰化各步反应的最佳反应温度和反应时间,分析了各组分间相互作用及其用量对衍生化效率的影响.对多种糖与糖醇乙酰化产物进行毛细管气相色谱分离、FID检测及GC-MS结构鉴定.研究证明,在合适条件下应用此方法对糖与糖醇进行乙酰化,反应完全,产物单一,能得到理想的分离、检测和定量分析效果.适用于微量植物组织中多种单糖、双糖及其糖醇的定量分析.

Gas Chromatographic Analysis of Sugar and Sugar Alcohol Derivatives Through 1-Methylimidazole Catalyzed Acetylation

Sugars and sugar alcohols are widely distributed natural compounds with high boiling and melting points. Chemical and instrumental analysis of sugars and sugar alcohols needs to derivate them into their derivatives. In this study, 1-methylimidazole was used as solvent and catalyst, hy- droxylamine hydrochloride and acetic anhydride were used as reagent for oximization and acetylation, respectively. The optimal temperature and time for the reaction of derivation were determined through the experiments. The effect of the components and the proper dosage of sugar and sugar alcohol were discussed. The products of the derivation reaction were separated effectively by gas chromatogra- phy with a capillary column, detected by a FID detector and structurally identified and characterized by GC-MS. The result of GC-FID and GC-MS shows that sugars and sugar alcohols can be acetylated completely under optimized conditions. The result of GC-FID analysis shows that sugars and sugar alcohols can be separated, detected and quantitatively determined.