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目的建立一种柱前衍生-超高效液相色谱法(ultra performance liquid chromatography,UPLC)检测香菇菌多糖片中单糖组成的分析方法。方法为排除香菇菌多糖片中辅料干扰,采用UPLC对香菇菌多糖原料中单糖组分进行定性分析,确定原料中的单糖组成。对超高效液相色谱法进行优化及方法学考察,以香菇菌多糖原料中主要单糖组成为依据对香菇菌多糖片单糖组成进行分析,确定香菇菌多糖片的单糖组成及摩尔比例。结果香菇菌多糖片的主要糖单元为甘露糖、葡萄糖和半乳糖,摩尔比为:4.6:4.28:6.375,方法学验证结果表明该单糖组成测定方法的精密度良好,样品中所测单糖的加样回收率为96.6%~103.8%,相对标准偏差在2.0%~2.6%之间,各单糖标准曲线线性相关系数大于0.999,线性关系良好。结论此方法快速、高效、准确,并为香菇菌多糖片的质量控制提供了保障。
OBJECTIVE To establish a method for the determination of monosaccharide composition in the polysaccharides of Lentinus edodes by ultra performance liquid chromatography (UPLC). Methods In order to exclude the interference of the excipients in the fungus mushroom polysaccharide tablets, UPLC was used to qualitatively analyze the monosaccharide components in the polysaccharides of the mushrooms, and to determine the monosaccharide composition in the raw materials. The ultra performance liquid chromatography was optimized and the methodological study was carried out. The monosaccharide composition of the polysaccharide from Lentinula edodes was analyzed based on the composition of the main monosaccharide in the raw material of Lentinula edodes polysaccharide, and the monosaccharide composition and the molar ratio of the polysaccharide from Lentinula edodes were determined. Results The main saccharide units of mushroom polysaccharide tablets were mannose, glucose and galactose, the molar ratio was 4.6: 4.28: 6.375. The methodological validation showed that the method of determination of the composition of monoglyceride was of good precision. The monosaccharide The recoveries were between 96.6% and 103.8%, with relative standard deviations between 2.0% and 2.6%. The linear correlation coefficients of each standard curve were above 0.999 and the linearity was good. Conclusion This method is rapid, efficient and accurate, and provides a guarantee for the quality control of mushroom polysaccharide tablets.