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对气相色谱法测定单糖时所用的毛细管色谱柱及单糖的预衍生化方法作了比较研究。在3种常用的衍生化方法中,选用了在盐酸羟胺及乙酸酐存在下将单糖转化成糖醛腈乙酰酯的衍生方法。试验了5种毛细管柱,其中以OV-1701及FFAP两种所得分离效果最好,且给出较对称的峰形,测定时用肌醇作内标。应用此方法测定了7种单糖,即L-鼠李糖、D-岩藻糖、D-阿拉伯糖、D-木糖、D-甘露糖、D-葡萄糖及D-半乳糖,其分析响应信号与浓度之间均保持一定的线性关系。7种单糖的检出限(3S/N)均小于14μg。在一已知样品中分别加入单糖的标准后检测方法的回收率,测得结果在92.5%～102.5%之间,精密度试验所测得的相对标准偏差(n=5)均小于2.5%。
A comparative study was made on capillary columns and pre-derivatization of monosaccharides used in the determination of monosaccharides by gas chromatography. Among the three commonly used derivatization methods, derivatization methods for converting monosaccharides to glucuronaldehyde acetyl esters in the presence of hydroxylamine hydrochloride and acetic anhydride were used. Five kinds of capillary columns were tested, of which OV-1701 and FFAP obtained the best separation effect, and gave a more symmetrical peak shape, using inositol as an internal standard. Using this method, seven monosaccharides, namely L-rhamnose, D-fucose, D-arabinose, D-xylose, D-mannose, D-glucose, and D-galactose, were analyzed. Both the signal and the concentration maintain a certain linear relationship. The limit of detection (3S/N) of the 7 monosaccharides was less than 14 μg. The recovery rate of the standard post-test method for monosaccharides was added to a known sample, and the result was between 92.5% and 102.5%. The relative standard deviation (n=5) measured in the precision test was less than 2.5%. .