Abstract The pyrolytic behaviour of two oligosaccharides – cellobiose and cellohexose – was studied using reactive pyrolysis-GC/MS with in situ hexamethyldisilazane derivatisation. Pyrolysis was conducted in a sealed vessel at various times ranging from 0.2 to 60 min. Semi-quantitative calculations were carried out on integrated peak areas to obtain information on derivatisation efficiency and composition of the pyrolysate as a function of pyrolysis time. The results were compared with a previous work by us in which glucose and cellulose were studied with the same procedure. The relative areas of anhydrosugars were found to decrease with the increase of the degree of polymerisation of the substrate, while the derivatisation efficiency showed an opposite trend. The results were explained by considering the role of both the sealed environment and water molecules freed during the pyrolysis process. We hypothesised that higher amounts of water were released from glucans with low degrees of polymerization, hindering both secondary pyrolysis reactions and derivatisation efficiency. Glucans with high degrees of polymerization, on the contrary, showed high signals of secondary pyrolysis products, consistent with a lower amount of water and the formation of a liquid phase.

中文翻译：

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作为热解时间函数的葡聚糖分析热解中的热解产物组成和硅烷化效率

摘要 使用反应热解-GC/MS 与原位六甲基二硅氮烷衍生化研究了两种低聚糖——纤维二糖和纤维己糖——的热解行为。热解在密封容器中进行，时间范围为 0.2 至 60 分钟。对积分峰面积进行半定量计算，以获得关于衍生效率和热解产物组成与热解时间的函数的信息。将结果与我们之前的工作进行了比较，在该工作中使用相同的程序研究了葡萄糖和纤维素。发现脱水糖的相对面积随着底物聚合度的增加而减少，而衍生效率则显示出相反的趋势。通过考虑密封环境和热解过程中释放的水分子的作用来解释结果。我们假设从低聚合度的葡聚糖中释放出更多的水，从而阻碍了二次热解反应和衍生效率。相反，具有高聚合度的葡聚糖显示出二次热解产物的高信号，与较低量的水和液相的形成一致。