OBJECTIVE:To establish a method for the content determination of diosmin crude drug and its tablets and related substances.METHODS:HPLC method was adopted.The determination was performed on Phenomenex C18 column (100 mm×4.6 mm,3 μm) with mobile phase consisted of water-methanol-acetic acid-acetonitrile (66∶28∶6∶2) at flow rate of 0.7 ml/min.The detection wavelength was set at 275 nm and column temperature was 40 ℃.RESULTS:The linear range of main component in related substances test were 2.47-98.9 μg/ml (r=0.999 9) and the limits of related impurity were 0.25％-10.0％; the linear range of hesperidin were 0.996-99.7 μg/ml (r=0.999 9) and the limits of related impurity were 0.1％-10.0％; the linear range of main components in content test were 99.63-298.9 μg/ml (r=0.999 9).Average recovery was 99.2％ (RSD=0.5％,n=6),and the limits of detection were 15 ng for diosmin and 5 ng for hesperidin.CONCLUSIONS:Same chromatographic system is used to determine the contents of main component and related substance in this method,improve quality standard and control the quality of diosmin crude drug and its tablets.%目的:建立测定地奥司明原料药及片剂的含量和有关物质的方法.方法:采用高效液相色谱法.色谱柱为Phenomenex C18(100 mm×4.6 mm,3 μmn),流动相为水-甲醇-冰醋酸-乙腈(66∶28∶6∶2),检测波长为275 nm,柱温为40℃,流速为0.7 ml/min.结果:有关物质中主成分检测质量浓度线性范围为2.47～98.9 μg/ml(r=0.999 9),相应的杂质限度范围为0.25％～10.0％;已知杂质橙皮苷的检测质量浓度线性范围为0.996～99.7 μg/ml(r=0.999 9),相应的杂质限度范围为0.1％～10.0％;含量测定中主成分检测质量浓度线性范围为99.63～298.9 μg/ml(r=0.999 9),平均回收率为99.2％ (RSD=0.5％,n=6);地奥司明、橙皮苷的检测限分别为15、5rng.结论:本方法采用同一色谱系统对地奥司明原料药及片剂的含量和有关物质进行了测定,完善了质量标准,可有效控制本品质量.
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