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目的对中华人民共和国药典一部(2015版)中铁皮石斛中甘露糖的含量测定方法进行讨论,简化已有方法的实验操作步骤。方法使用超声提取法代替索氏提取法去除铁皮石斛样品中的游离单糖,使用微波法代替煎煮法提取样品中的甘露糖,去除衍生反应和内标法定量步骤。样品提取液经微孔滤膜过滤后,采用药典中的高效液相色谱法分析,外标法定量分析甘露糖的含量。结果甘露糖在0.054~0.648 mg/mL的浓度范围内与峰面积呈良好的线性关系,相关系数r>0.999。甘露糖在3个不同添加水平下的平均回收率分别为97.66%、98.10%和98.68%。结论本方法大大缩短了样品的前处理时间,操作简便、准确度和精密度良好,可以用于铁皮石斛中甘露糖的含量测定。
Objective To discuss the method of determination of mannose in Dendrobium officinale from the first edition of Pharmacopoeia of the People’s Republic of China (2015 edition), and to simplify the experimental procedures of the existing methods. Methods Ultrasound extraction method was used to replace Soxhlet extraction to remove free monosaccharide in Dendrobium officinale samples. The microwave method was used to replace mannose extraction in the decoction method to remove the derivatization reaction and the internal standard method. The sample extract was filtered through a microporous membrane filter, using high performance liquid chromatography in the Pharmacopoeia, external standard method for quantitative analysis of mannose content. Results Mannose showed a good linear relationship with the peak area in the range of 0.054 ~ 0.648 mg / mL with the correlation coefficient r> 0.999. The average recoveries of mannose at three different added levels were 97.66%, 98.10% and 98.68%, respectively. Conclusion This method greatly shortens the sample pretreatment time, easy operation, accuracy and precision, can be used for determination of mannose content in Dendrobium officinale.