苗药金铁锁质量标准完善研究

目的: 控制金铁锁药材质量,完善2010年版中国药典中金铁锁药材质量标准,优化浸出物测定项,建立显微横切面鉴别和含量测定标准。方法: 采用横切面及粉末显微法、正相分配薄层色谱法进行鉴别;采用中国药典附录方法,对水分、总灰分、浸出物进行测定;采用HPLC法测定酸水解后金铁锁皂皮酸苷元的含量,色谱柱为Zorbax Eclipse Plus C₁₈ (250 mm×4.6 mm,5 μm),流 动相为乙腈-水,梯度洗脱,流速1.0 mL · min^-1,柱温25 ℃,检测波长210 nm。结果: 金铁锁横切面和粉末的显微特征与文献描述基本一致;薄层色谱斑点清晰,分离好;含量测定皂皮酸进样量在1.049~20.98 μg范围内线性关系良好(r=0.999 9),平均回收率为98.4%(RSD为3.0%,n=6),皂皮酸含量不低于0.10%。结论: 本文优化后的浸出物测定方法以及建立的显微横切面鉴别和含量测定方法可为进一步完善金铁锁药材质量标准提供依据。

Objective: To control the quality of the Miao ethnic herb Psammosilenes Radix by establishing standards of transverse section identification and assay, optimizing determination items of extractives and improving quality standards of Psammosilenes Radix in Chinese Pharmacopoeia(2010 version). Methods: Microscopical characteristics were studied based on transverse section and powder.Normal phase TLC was adopted to identify Psammosilenes Radix.Water, total ash and extractives were determined by methods described in appendices of Chinese Pharmacopoeia.The quillaic acid of total saponins after acid hydrolysis was determined by HPLC.The Agilent Zorbax Eclipse Plus C₁₈ (250 mm×4.6 mm, 5 μm)column was used, the mobile phase was acetonitrile-water at the flow rate of 1 mL · min^-1, the column temperature was 25 ℃ and the detection wavelength was at 210 nm. Results: Microscopical characteristics of transverse section and powder were in good accordance with the records in Chinese Pharmacopoeia(2010 version, volume Ⅰ)and literatures.The TLC showed the spots developed clearly and the separation was good.The concentration of quillaic acid showed a good linear relationship in the range of 1.049-20.98 μg(r=0.9999), and the average recovery was 98.4%(RSD was 3.0%, n=6), the limit of quillaic acid content was set as not less than 0.10%. Conclusion: This paper optimized the extractive-measuring method, established the microscopic transverse section identification and content determination method, which could provide evidence for further improvement of quality standards of Psammosilenes Radix.