明目地黄丸(浓缩丸)质量标准研究

Quality standard for Mingmu Dihuang Pills(concentrated pills)

目的制定明目地黄丸(浓缩丸)(熟地黄、当归、酒萸肉、牡丹皮、白芍、山药、枸杞子、菊花等)的质量标准。方法采用薄层色谱法对明目地黄丸(浓缩丸)中的牡丹皮、当归、白芍、熟地黄等进行定性鉴别;HPLC法测定明目地黄丸(浓缩丸)中马钱苷、丹皮酚和芍药苷。马钱苷色谱条件:色谱柱为Kromasil C18(250 mm×4.6mm,5μm),流动相为四氢呋喃-乙腈-甲醇(1∶8∶4)-0.05%磷酸溶液(8∶92),检测波长为236 nm,体积流量为1.0mL/min;丹皮酚色谱条件:色谱柱为Agilent Zorbax SB-C18(250 mm×4.6 mm,5μm),流动相为甲醇-水(48∶52),检测波长为274 nm,体积流量为1.0 mL/min;芍药苷色谱条件:色谱柱为Agilent Zorbax C18(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸溶液(14∶86),检测波长为230 nm,体积流量为1.0 mL/min。结果处方中当归、牡丹皮、芍药苷的薄层色谱鉴别专属性较强。马钱苷、丹皮酚和芍药苷分别在40.43～1 213.02 ng、40.43～1 213.02 ng和40.43～1 213.02 ng范围内线性关系良好(r均为1.000 0),平均回收率分别为96.4%(n=6),98.2%(n=6)和98.3%(n=6);RSD值分别为0.8%,0.8%和2.1%。结论本研究所建立的方法简便快速,准确可靠,可有效控制明目地黄丸(浓缩丸)的质量。

AIM To establish the quality standard for Mingmu Dihuang Pills（concentrated pills）（Rehmanniae Radix praeparata,Angelicae sinensis Radix,Corni Fructus,Moutan Cortex,Paeoniae Radix alba,Dioscoreae Rhizoma,Lycii Fructus,Chrysanthemi Flos,etc.）.METHODS Moutan Cortex,Angelicae sinensis Radix,Paeoniae Radix alba,Rehmanniae Radix praeparata,etc.in the formulation were qualitatively identified by TLC.The contents of loganin,paeonol and peoniflorin were analyzed by HPLC.The analyses of the three components were performed on a Kromasil C18 and Agilent Zorbax SB-C18column（250 mm×4.6 mm,5 μm） with tetrahydrofuran-acetonitrile-methanol（1∶8∶4）-0.05% phosphoric acid solution（8∶92）,methanol-water（48∶52） and acetonitrile-0.1% phosphoric acid solution（14∶86） as mobile phase respectively at a flow rate of 1.0 mL/min.The detection wavelengths were at 236,274 and 230 nm,respectively.RESULTS There were good specificities of TLC for Moutan Cortex,Angelicae sinensis Radix and peoniflorin.The linear ranges of loganin,paeonol and peoniflorin were 40.43-1 213.02 ng,40.43-1 213.02 ng and 40.43-1 213.02 ng,respectively（r=1.000 0）.The average recoveries were 96.4%,98.2% and 98.3%,respectively and RSDs were 0.8%,0.8% and 2.1%,respectively.CONCLUSION The methods established in the study are simple,accurate,reliable and suitable to be applied to the quality control for the preparation.