摘要
目的建立一测多评法,同时测定清热疏肝口服液中氧化芍药苷、芍药苷、滨蒿内酯、金丝桃苷、异槲皮苷、4,5-O-二咖啡酰奎宁酸、柴胡皂苷a和柴胡皂苷d的含量。方法以Waters Symmetry C 18柱(250 mm×4.6 mm,5μm)为色谱柱,柱温:30℃;流动相:乙腈-0.1%磷酸水溶液,梯度洗脱,流速:1.0 ml/min;检测波长分别为230 nm(检测氧化芍药苷、芍药苷)、345 nm(检测滨蒿内酯、金丝桃苷、异槲皮苷、4,5-O-二咖啡酰奎宁酸)和210 nm(检测柴胡皂苷a、柴胡皂苷d)。以异槲皮苷为内参物,建立其与氧化芍药苷、芍药苷、滨蒿内酯、金丝桃苷、4,5-O-二咖啡酰奎宁酸、柴胡皂苷a和柴胡皂苷d的相对校正因子,通过相对校正因子计算清热疏肝口服液中上述7种成分含量,比较计算值与外标法实测值的差异。结果氧化芍药苷、芍药苷、滨蒿内酯、金丝桃苷、异槲皮苷、4,5-O-二咖啡酰奎宁酸、柴胡皂苷a和柴胡皂苷d分别在1.29~25.80、6.96~139.20、5.78~115.60、2.47~49.40、0.88~17.60、8.71~174.20、2.09~41.80、1.76~35.20μg/ml范围内线性关系良好(r≥0.9994),平均加样回收率(RSD)分别为98.27%(1.50%)、99.00%(0.53%)、99.82%(0.81%)、97.93%(1.44%)、97.68%(1.16%)、100.04%(0.64%)、98.90%(0.97%)和96.86%(1.09%);氧化芍药苷、芍药苷、滨蒿内酯、金丝桃苷、4,5-O-二咖啡酰奎宁酸、柴胡皂苷a和柴胡皂苷d的相对校正因子分别为0.3672、0.4628、0.5355、0.3180、0.5176、0.3398、0.3840,其计算值和实测值之间无明显差异。结论该方法操作便捷、结果准确、重复性好,可用于清热疏肝口服液中8种活性成分的同时测定。
Objective To establish the method of quantitative analysis of multi-components by single marker(QAMS)for the simultaneous determination of oxypaeoniflorin,paeoniflorin,scoparone,hyperoside,isoquercitrin,4,5-O-dicaffeoyl quinic acid,saikosaponin a and saikosaponin d in Qingre Shugan Koufuye.Methods The determination was performed on a Waters Symmetry C 18(250 mm×4.6 mm,5μm)column with the mobile phase consisting of acetonitrile-0.1%phosphoric acid aqueous solution and the gradient elution at the flow rate of 1.0 ml/min.The column temperature was set at 30℃.The detection wavelength was set at 230 nm for oxypaeoniflorin and paeoniflorin,345 nm for scoparone,hyperoside,isoquercitrin and 4,5-O-dicaffeoyl quinic acid,and 210 nm for saikosaponin a and saikosaponin d.Using scoparone as the internal standard,an HPLC method was used to calculate the relative correction factor(RCF)of scoparone to oxypaeoniflorin,paeoniflorin,hyperoside,isoquercitrin,4,5-O-dicaffeoyl quinic acid,saikosaponin a and saikosaponin d.The contents of the above-mentioned 7 components in Qingre Shugan Koufuye were calculated by using RCF.The differences between the calculation values and the measured values by external standard method were compared.Results Oxypaeoniflorin,paeoniflorin,scoparone,hyperoside,isoquercitrin,4,5-O-dicaffeoyl quinic acid,saikosaponin a and saikosaponin d showed good linear relationships within the ranges of 1.29~25.80,6.96~139.20,5.78~115.60,2.47~49.40,0.88~17.60,8.71~174.20,2.09~41.80 and 1.76~35.20μg/ml(r≥0.9994),whose average recoveries(RSD)were 98.27%(1.50%),99.00%(0.53%),99.82%(0.81%),97.93%(1.44%),97.68%(1.16%),100.04%(0.64%),98.90%(0.97%)and 96.86%(1.09%),respectively.RCFs of scoparone to oxypaeoniflorin,paeoniflorin,hyperoside,isoquercitrin,4,5-O-dicaffeoyl quinic acid,saikosaponin a and saikosaponin d were 0.3672,0.4628,0.5355,0.3180,0.5176,0.3398 and 0.3840,respectively.There were no significant differences between the calculated values and the measured values.Conclusion The method is simple and accurate with good repeatability,which can be used for the simultaneous determination of 8 active components in Qingre Shugan Koufuye.
作者
刘艳芬
马云
LIU Yan-fen;MA Yun(Department of Pharmacy,Southern Hospital,Southern Medical University,Guangzhou 510515,China)
出处
《实用药物与临床》
CAS
2020年第9期836-841,共6页
Practical Pharmacy and Clinical Remedies
关键词
一测多评法
清热疏肝口服液
相对校正因子
含量测定
Quantitative analysis of multi-components by single-marker(QAMS)
Qingre Shugan Koufuye
Relative correction factor
Content determination
