铁皮石斛中甘露糖的提取与检测方法优化

摘要

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 detection method of mannose inDendrobium officinale Kimuraet Migo in harmacopoeia of People’s Republic of China Part I (2005 Edition) and simplify the operation steps of existing method. MethodsThe free monosaccharide inDendrobium officinale Kimuraet Migo samples was removed by ultrasonic extraction method instead of soxhlet extraction, and the mannose in samples was extracted by microwave method instead of dew decoction method. There was no derivative reaction and internal standard method in this method. The sample extract was filtered by microporous filtering film, then analyzed by the high performance liquid chromatography (HPLC) described in harmacopoeia, and the content of mannose was determined by external standard method.Results There was a good linear relationship between the mannose content which ranged from 0.054~0.648 mg/mL and peak area with the correlation coefficient (r) greater than 0.999. The average recoveries of mannose at 3 different adding levels were 97.66%, 98.10% and 98.68%, respectively.Conclusion This method is simple, accurate, precise, and greatly shorten the processing time, which can be used to the content determination of mannose in Dendrobium officinale Kimuraet Migo.