摘要
目的 建立健脾止泻胶囊多糖的含量测定方法。方法以无水葡萄糖为对照品,采用苯酚-硫酸法测定总糖含量;采用1.5 mol/L硫酸溶液水解多糖,通过碱中和、乙醇沉淀的方法得到单糖,用HPLC-ELSD方法测定其含量;色谱条件:色谱柱为Xbridge Amide column(4.6 mm×150 mm,3.5μm);流动相为乙腈∶0.1%三乙胺(75∶25);柱温:30℃;流速为1.0 m L/min;ELSD漂移管温度为95℃;气体流速为3.0 L/min。结果苯酚-硫酸法中,葡萄糖在6.8~68.0μg/m L范围内与吸光度呈良好的线性关系(r2=0.9995),平均回收率为96.1%。HPLC-ELSD法中,无水葡萄糖在0.0507~0.8110 mg/m L范围内呈现良好的线性关系(r2=0.9998),平均回收率为97.1%,RSD为1.4%。两种测定方法测定多糖的平均含量分别为22.3%、15.2%。结论该方法稳定可行,重复性好,可以作为健脾止泻胶囊多糖的含量测定方法。
Objective To establish a determination method for polysaccharide in Jianpizhixie Capsules Methods Anhydrous glucose was used as reference substance. Total sugar content was determined by phenol-sulfate acid method;1.5mol/L hydrolyzed polysaccharide sulfate solution was used, the method of alkali neutralization and ethanol precipitation was used to get simple sugars. The HPLC-ELSD method was used to determine its content. Chromatographic condition: chromatographic column was Xbridge Amide column(4.6 mm×150 mm, 3.5 μm); Mobile phase was acetonitrile-0.1% triethylamine(75 ∶25), column temperature was 30℃, flow rate was 1.0 m L/min, temperature of ELSD was95℃, gas flow rate was 3.0 L/min. Results Phenol-sulfate acid method of anhydrous glucose was linear in the ranges of6.8-68.0 μg/m L(r2= 0.9995), the average recovery rate was 96.1%. HPLC-ELSD of anhydrous glucose was linear in the ranges of 0.0507-0.8110 mg/m L(r2= 0.9998), the average recovery was 97.1%, RSD = 1.4%. The average contents of two kinds methods for determination of polysaccharide were 22.3%, 15.2%. Conclusion The method is stable and feasible, has good repeatability and can be used as the polysaccharide content determination of Jianpizhixie Capsules.
出处
《中国医药导报》
CAS
2016年第3期39-43,共5页
China Medical Herald
