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作 者:王贤儿 钟希文[2] 曾聪彦[2] 汪亚飞[1] 张文霞[2]
机构地区:[1]广州中医药大学,广东广州510006 [2]广州中医药大学附属中山中医院,广东中山528400
出 处:《中成药》2014年第9期1867-1872,共6页Chinese Traditional Patent Medicine
基 金:中山市科技局科技计划资助项目(20132A161)
摘 要:目的建立蛇黄散(蛇鳞草、大黄、三角草、山芝麻和独行千里)的质量标准。方法 TLC法鉴定方中蛇鳞草、大黄、三角草、山芝麻;采用HPLC法测定三羽新月蕨苷A、大黄酸以及大黄素的量,色谱柱为Boston Green ODS C18(4.6 mm×250 mm,5μm),流动相为乙腈-甲醇-0.1%磷酸水溶液,梯度洗脱,体积流量1 mL/min,检测波长为226 nm。结果薄层鉴别色谱中特征斑点明显,重复性较好。三羽新月蕨苷A在0.016~0.128 mg/mL范围内线性关系良好(r=0.999 9),平均回收率为100.5%,RSD为1.6%(n=6);大黄酸在0.008~0.064 mg/mL范围内线性关系良好(r=0.999 9),平均回收率为99.4%,RSD为1.1%(n=6);大黄素在0.012~0.096 mg/mL范围内线性关系良好(r=0.9999),平均回收率为99.3%,RSD为1.9%(n=6)。结论本法采用的HPLC流动相能改善三羽新月蕨苷A色谱峰拖尾现象。AIM To establish a quality standard for Shehuang Powder (Pronephrium triphyllum , Rhei Radix et Rhizoma , Chlorophytum laxum R. Br and Helicteres angustifolia L ). METHODS P. triphyllum, Rhei Ra- dix et Rhizoma, C. laxum R. Br and H. angustifolia L. were identified by TLC. The contents of triphyllinA, rhein and emodin were determined by HPLC. The HPLC analysis was performed on Boston Green ODS Cls (4. 6 mm × 250 mm, 5 μm), mobile phase consisted of acetonitrile-methanol-0. 1% phosphoric acid in a gradient elu- tion manner with the flow rate of 1.0 mL/min and detection wavelength of 226 nm. RESULTS Characteristic spots could be detected by TLC and the method had good reproducibility. Triphyllin A was linear in the range of 0. 016 × 0. 128 mg/mL ( r =0. 999 9). The average recovery rate was 100. 5% and RSD was 1.6% ( n =6). Rhein was linear in the range of 0. 008 - 0. 064 mg/mL ( r = 0. 999 9 ). The average recovery rate was 99.4% and RSD was 1.1% (n=6). Emodin was linear in the range of 0. 012 -0. 096 mg/mL ( r=0. 999 9 ). The average recovery rate was 99.3% and RSD was 1.9% ( n = 6) . CONCLUSION Mobile phase developed can improve tailed peak of triphyllin A in HPLC analysis.
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