扶正解毒散中淫羊藿鉴别方法研究

Study on the Identification Method of Epimedium in Fuzhengjiedu Mixture

为更加准确地控制扶正解毒散中淫羊藿的鉴别,建立扶正解毒散中淫羊藿的鉴别方法和淫羊藿苷的含量测定方法;将乙酸乙酯、甲酸、水、丁酮按照20∶2∶2∶2比例混合均匀,以此混合液作为展开剂,展开后用三氯化铝试液均匀喷涂薄层板,置于干燥箱内80℃烘烤5 min,然后置于365 nm波长的紫外灯下检视;该条件下,供试品、淫羊藿对照药材和淫羊藿苷对照品在相同的位置上具有相同颜色的斑点,并且该方法的分离度好,阴性对照无干扰。液相色谱条件:Supersil ODS2柱(4.6 mm×250 mm,5μm),以30%乙腈和70%水混合后的均匀液体作为流动相;流速1.0 mL/min;柱温30℃;检测波长270 nm;进样体积10μL。淫羊藿苷线性回归方程为Y=22109X﹣368.12(r=0.9997,n=5),淫羊藿苷在10.0~80.0μg/mL范围内线性关系良好。试验建立的淫羊藿鉴别方法和含量测定方法具有操作简便,结果稳定的优点,更有利于控制扶正解毒散的质量稳定。

To establish the TLC and HPLC for content of Fuzhengjiedu Mixture.TLC condition:Ethyl acetate-butanone-formic acid-water(20∶2∶2∶2)was used as the developing agent.Unfolding with the developing agent and spraying Aluminium trichloride solution.Heating at 80℃for5 min,checking under 365 nm uv lamp.The results showed that under this condition,the fluorescent spots of the sample were clear and the separation degree was good.Contrast herb of epimedium and reference substance have the same color and position of fluorescent spots.The negative control without interference.Liquid chromatographic condition:chromatographic column was Supersil ODS2(4.6 mm×250 mm,5μm),The mobile phase was 70%acetonitrile and 30%water.The flow rate is 1.0m L/min,column temperature was 30℃,the detection wavelength is 270 nm and injection volume is 10 liters.The linear regression equation of icariin is Y=22109X-368.12(r=0.9997,n=5).The linear relationship in 10.0~80.0μg/mL was good.The method is simple,accurate with strong specificity and can be used for the quality control of Fuzhengjiedu Mixture.