Glycosyl linkage (methylation) analysis is used widely for the structural determination of oligo- and poly-saccharides. The procedure involves derivatisation of the individual component sugars of a polysaccharide to partially methylated alditol acetates which are analysed and quantified by gas chromatography-mass spectrometry. The linkage positions for each component sugar can be determined by correctly identifying the partially methylated alditol acetates. Although the methods are well established, there are many technical aspects to this procedure and both careful attention to detail and considerable experience are required to achieve a successful methylation analysis and to correctly interpret the data generated. The aim of this article is to provide the technical details and critical procedural steps necessary for a successful methylation analysis and to assist researchers (a) with interpreting data correctly and (b) in providing the comprehensive data required for reviewers to fully assess the work.

糖基键（甲基化）分析被广泛用于寡糖和多糖的结构测定。该程序包括将多糖的各个成分糖衍生为部分甲基化的糖醇乙酸酯，然后通过气相色谱-质谱法对其进行分析和定量。每个糖成分的键合位置可以通过正确鉴定部分甲基化的糖醇乙酸酯来确定。尽管这些方法已经很好地建立了，但是此过程有很多技术方面，要成功进行甲基化分析并正确解释生成的数据，既需要仔细注意细节，也需要丰富的经验。