摘要
目的 建立一测多评法同时测定五灵胶囊中柴胡皂苷a、柴胡皂苷d、五味子甲素、五味子乙素、五味子醇甲、丹参酮ⅡA、丹酚酸B、隐丹参酮的含量.方法 采用高效液相色谱法,色谱柱为Agilent ZORBAX SB-C18色谱柱(4.6 mm×250 mm,5 μm);流动相为乙腈-0.1％磷酸溶液,梯度洗脱;流速1.0 ml/min;检测波长210 nm;柱温30℃.以五味子醇甲为内参物,建立柴胡皂苷a、柴胡皂苷d、五味子甲素、五味子乙素、丹参酮ⅡA、丹酚酸B、隐丹参酮的相对校正因子;计算8种成分的含量,并与外标法测定结果进行对比分析.结果 柴胡皂苷a、柴胡皂苷d、五味子甲素、五味子乙素、五味子醇甲、丹参酮ⅡA、丹酚酸B、隐丹参酮分别在9.58～191.50,9.10～182.02,1.04～25.89,2.00～50.10,5.37～134.35,1.00～25.08,8.27～206.72,1.07～26.67 µg/ml范围内线性关系良好(r≥0.9992);精密度、重复性、稳定性实验RSD均小于2％;平均加样回收率为97.06％～99.95％,RSD为0.53％～1.73％.一测多评法与外标法测定结果一致.结论 该方法简便、准确,可用于五灵胶囊的质量评价.
Abstract
Objective To establish a method for simultaneous determination of saikosaponin a,saikosaponin d,schisandrin A,schisandrin B,schisandrol A,tanshinone ⅡA,salvianolic acid B and cryptotanshinone in Wuling Capsules by quantitative analysis of multi-components by single marker(QAMS).Methods The HPLC separation was achieved on an Agilent ZORBAX SB-C18 column(4.6 mm×250 mm,5 μm)with acetonitrile-0.1％phosphoric acid as mobile phase of gradient elution,which was at a flow rate of 1.0 ml/min.The determination wavelength was 210 nm.The column temperature was set at 30℃.With schisandrol A as the internal reference,the relative correction factors of saikosaponin a,saikosaponin d,schisandrin A,schisandrin B,tanshinone ⅡA,salvianolic acid B and cryptotanshinone were calculated.The contents of 8 components were calculated and compared with those determined by the external standard method(ESM).Results Saikosaponin a,saikosaponin d,schisandrin A,schisandrin B,schisandrol A,tanshinone ⅡA,salvianolic acid B and cryptotanshinone showed good linear relationships within the ranges of 9.58-191.50,9.10-182.02,1.04-25.89,2.00-50.10,5.37-134.35,1.00-25.08,8.27-206.72,1.07-26.67 µg/ml(r≥0.9992).RSDs of precision,repeatability and stability tests were all less than 2％.The average recoveries were 97.06％-99.95％,with the RSDs of 0.53％-1.73％.The results of QAMS were consistent with those of ESM.Conclusion The method is simple and accurate,and can be used to evaluate the quality of Wuling Capsules.
维普
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