Kennedy J F, Robertson S M, Stacey M
Carbohydr Res. 1976 Jul;49:243-58. doi: 10.1016/s0008-6215(00)83142-0.
The free acids, sodium salts, and lactones of several hexuronic acids have been studied as their O-trimethylsilyl derivatives by gas-liquid chromatography using SE-30 and XE-60 liquid phases. Silylation was best performed in methyl sulphoxide. The equilibrium between the various forms of a hexuronic acid in methyl sulphoxide was also studied by g.l.c. following silylation. The hexamethyldisilazane used in the silylation disturbed the equilibrium attained in the solvent, but this was overcome by premixing the hexamethyldisilazane with chlorotrimethylsilane. Methyl sulphoxide and the silylating reagents gave a two-phase system in which the derivative was favourably partitioned into the upper layer. Partition coefficients and stabilities of the derivatives were measured, and a g.l.c. method for the analysis of the hexuronic acids was thereby developed. The oximes of the hexuronic acids were studied as alternative derivatives for g.l.c., and their equilibrium compositions and g.l.c. retention times are recorded.
几种己糖醛酸的游离酸、钠盐和内酯已作为它们的O-三甲基硅烷基衍生物，使用SE-30和XE-60固定相通过气液色谱法进行了研究。硅烷化最佳在二甲亚砜中进行。在硅烷化后，还通过气液色谱法研究了己糖醛酸在二甲亚砜中各种形式之间的平衡。硅烷化中使用的六甲基二硅氮烷扰乱了在溶剂中达到的平衡，但通过将六甲基二硅氮烷与三甲基氯硅烷预混合克服了这一问题。二甲亚砜和硅烷化试剂形成了一个两相体系，其中衍生物有利地分配到上层。测量了衍生物的分配系数和稳定性，从而开发了一种用于分析己糖醛酸的气液色谱法。研究了己糖醛酸的肟作为气液色谱法的替代衍生物，并记录了它们的平衡组成和气液色谱保留时间。
