本文对制备单糖三甲基硅醚衍生物的条件进行了考察。同时提出在单糖进行硅醚化反应后适量加水的简易后处理方法,能显著减少色谱测定时溶剂峰的“拖尾”,并消除了反应后产生的沉淀。在测定单糖结晶样品时,采用加溶剂后迅速加入硅醚化试剂的方法,能有助于使单糖衍生物得到单峰。本实验提供了阿拉伯糖、木糖、果糖、山梨糖、葡萄糖结晶样品三甲基硅醚衍生物适宜的气相色谱分析条件。 In this paper, the conditions for preparing monosaccharide trimethylsilyl ether derivatives were investigated. At the same time, a simple post-treatment method of adding proper amount of water after the silyl etherification reaction of monosaccharides is proposed, which can significantly reduce the “tailing” of the solvent peak during the chromatographic determination and eliminate the precipitation after the reaction. In the determination of monosaccharide crystallization samples, the method of adding the silicon ether reagent quickly after adding the solvent can help to make the monosaccharide derivative to obtain a single peak. This experiment provided suitable conditions for gas chromatographic analysis of trimethylsilyl ether derivatives of arabinose, xylose, fructose, sorbose and glucose crystals.