宁心安神颗粒定性定量方法研究
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摘要
目的建立宁心安神颗粒的定性定量方法。方法采用薄层色谱法(TLC)对方中的炒酸枣仁、刺五加和夏枯草进行定性鉴别;以高效液相色谱法(HPLC)分别测定制剂中酸枣仁皂苷A和紫丁香苷的含量,酸枣仁皂苷A的含量测定采用Agilent C_(18)色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-水,流速为1.0 mL·min~(-1),蒸发光检测器,雾化温度60℃,柱温为25℃;紫丁香苷的含量测定采用Agilent C_(18)色谱柱(4.6 mm×250 mm,5μm),流动相为甲醇-水,流速为1.0 mL·min~(-1),检测波长265 nm,柱温为25℃。结果炒酸枣仁、刺五加和夏枯草的TLC图斑点清晰,分离度较好且阴性样品无干扰;酸枣仁皂苷A、紫丁香苷的线性范围分别为72.1～1154.3μg·mL~(-1)(r=0.9999),4.5～90.8μg·mL~(-1)(r=0.9997),仪器精密度和重复性试验的RSD均小于2%,平均加样回收率分别为103.5%、95.6%。结论本试验所建立的方法专属性强,准确可靠,可用于宁心安神颗粒的质量控制。
Objective To establish the qualitative and quantitative method of compound Ningxin Anshen granules.Methods Thin layer chromatography(TLC) was used for the qualitative identification of fried Ziziphispinosaesemen,Acanthopanax senticosus radix et rhizoma seucaulis and Prunella vulgaris. The HPLC of spinosin was performed on Agilent C_(18) column(4.6 mm×250 mm, 5 μm) with the mobile phase consisting of acetonitrile-water at 1.0 mL·min~(-1),evaporative light-scattering detector, atomization temperature at 60 ℃, and the column temperature at 25 ℃. The HPLC of alkaloids was performed on Agilent column(4.6 mm×250 mm, 5 μm) with the mobile phase consisting of ethanol-water at 1.0 mL·min~(-1). The detection wavelength was 265 nm, and the column temperature was 25 ℃.Results The TLC plots of fried Ziziphispinosaesemen, Acanthopanacis senticosi radix et rhizoma seucaulis and Prunellae spica were clear and well resolved, with negative sample without interference. The jujube saponin A and syringin revealed a good linear relationship at 72.1-1154.3 μg·m L~(-1)(r = 0.9999), and 4.5-90.8 μg·m L~(-1)(r= 0.9997), respectively. The RSDs of precision, stability and repeatability were less than 2%. The average recoveries of the 2 components in Ningxin Anshen granules were 103.5% and 95.6%, respectively. Conclusion The method is specific and accurate, and can be used for the quality control of Ningxin Anshen granules.
Objective To establish the qualitative and quantitative method of compound Ningxin Anshen granules.Methods Thin layer chromatography(TLC) was used for the qualitative identification of fried Ziziphispinosaesemen,Acanthopanax senticosus radix et rhizoma seucaulis and Prunella vulgaris. The HPLC of spinosin was performed on Agilent C_(18) column(4.6 mm×250 mm, 5 μm) with the mobile phase consisting of acetonitrile-water at 1.0 mL·min~(-1),evaporative light-scattering detector, atomization temperature at 60 ℃, and the column temperature at 25 ℃. The HPLC of alkaloids was performed on Agilent column(4.6 mm×250 mm, 5 μm) with the mobile phase consisting of ethanol-water at 1.0 mL·min~(-1). The detection wavelength was 265 nm, and the column temperature was 25 ℃.Results The TLC plots of fried Ziziphispinosaesemen, Acanthopanacis senticosi radix et rhizoma seucaulis and Prunellae spica were clear and well resolved, with negative sample without interference. The jujube saponin A and syringin revealed a good linear relationship at 72.1-1154.3 μg·m L~(-1)(r = 0.9999), and 4.5-90.8 μg·m L~(-1)(r= 0.9997), respectively. The RSDs of precision, stability and repeatability were less than 2%. The average recoveries of the 2 components in Ningxin Anshen granules were 103.5% and 95.6%, respectively. Conclusion The method is specific and accurate, and can be used for the quality control of Ningxin Anshen granules.
引文
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[13]刘光兰,魏鲜娥,吴银,等.高效液相色谱法同时测定紫丁香苷、绿原酸、栀子苷和红景天苷的含量[J].食品安全质量检测学报,2017,8(12):4847-4853.
[2]刘朋朋.酸枣仁化学成分及其四种皂苷含量测定研究[D].北京:北京中医药大学,2013.
[3]耿欣,李廷利.酸枣仁主要化学成分及药理作用研究进展[J].中医药学报,2016,44(5):84-86.
[4]邵晓虹.酸枣仁汤镇静催眠有效部位群的筛选及其配伍研究[D].武汉:湖北中医药大学,2014.
[5]杨晓丹,井月娥,卢芳.刺五加的化学成分研究进展[J].中华中医药学刊,2015,33(2):316-318.
[6]樊如强,傅宏征,金学英,等.刺五加有效成分提取工艺考察及不同产地刺五加中有效成分量的比较[J].中草药,2014,45(2):260-264.
[7]赵敏.刺五加分散片的研制[D].长春:吉林大学,2015.
[8]黄明霞,邹堃,贺凯,等.夏枯草颗粒质量标准提高的实验研究[J].宁夏医学杂志,2016,38(4):329-331.
[9]刘婧姝,乔卫,郝兰芳,等.酸枣仁合欢方中酸枣仁皂苷A的薄层色谱鉴别和含量测定[J].中国实验方剂学杂志,2011,17(5):77-79.
[10]中国药典2015年版.四部[S]. 2015:57.
[11]牛春燕.酸枣仁中黄酮类化学成分及质量分析方法研究[D].北京:中国协和医科大学,2010.
[12]杨红.刺五加胶囊中紫丁香苷含量的HPLC测定[J].时珍国医国药,2013,24(2):404-405.
[13]刘光兰,魏鲜娥,吴银,等.高效液相色谱法同时测定紫丁香苷、绿原酸、栀子苷和红景天苷的含量[J].食品安全质量检测学报,2017,8(12):4847-4853.