铁皮石斛复方胶囊中甘露糖的含量检测方法研究

Study on Detecting Method of Mannose in Dendrobium officinale Compound Capsules

目的:建立通过高效液相色谱法(HPLC)测定铁皮石斛复方胶囊中甘露糖的方法。方法:样品以盐酸氨基葡萄糖为内标,分别经索式提取、盐酸水解和衍生化处理。采用Agilent Eclipse XDB-C18(4.6 mm×250 mm,5μm)色谱柱,以20 mmol·L^(-1)乙酸铵-乙腈溶液(83∶17)为流动相,流速1.0 mL·min^(-1),进样量10μL,波长250 nm,在室温下进行检测。结果:甘露糖在21.54~215.40μg·mL^(-1)(R^(2)=0.9999)范围内呈现良好的线性关系;其精密度实验的RSD值为0.22%,其重复性实验的RSD值为2.31%,其平均加样回收率为100.34%,RSD为2.46%。结论:供试品溶液在48 h内稳定,该方法专属性高、重复性好,可用于铁皮石斛复方胶囊中甘露糖的含量测定。本实验为铁皮石斛复方胶囊的质量标准制定提供了基础数据。

Objective:To establish a method for the determination of mannose in Dendrobium officinale compound capsules by high performance liquid chromatography(HPLC).Method:The samples were treated with Soxhlet extraction,hydrochloric acid hydrolysis and derivatization with glucosamine hydrochloride as the internal standard.Using Agilent Eclipse XDB-C18(4.6 mm×250 mm,5μm)chromatographic column,using 20 mmol·L^(-1) ammonium acetate-acetonitrile solution(83∶17)as mobile phase,flow rate 1.0 mL·min^(-1),injection The volume is 10μL,the wavelength is 250 nm,and the detection is performed at room temperature.Reaults:Mannose showed a good linear relationship in the range of 21.54~215.40μg·mL^(-1)(R^(2)=0.9999);the RSD value of the precision experiment was 0.22%,and the RSD value of the repeatability experiment was 2.31%.The average recovery rate was 100.34%,and the RSD was 2.46%.Conclusion:The test solution is stable within 48 hours.This method is highly specific and reproducible.It can be used for the determination of mannose in Dendrobium officinale compound capsules.This experiment provides basic data for the quality standard formulation of Dendrobium officinale compound capsules.