State Key Laboratory of Natural Products and Functions, China Pharmaceutical University, Nanjing 210009, China.
Chin J Nat Med. 2013 Jul;11(4):419-26. doi: 10.1016/S1875-5364(13)60063-1.
To study the related impurities in asperosaponin VI bulk drug and to develop a high performance liquid chromatography (HPLC) method for the determination of asperosaponin VI and its related impurities.
The related impurities were detected in asperosaponin VI bulk drug by a newly developed HPLC method, obtained by ODS column chromatography and semi-preparative HPLC methods, and the structures were elucidated by TOF-MS, IR, and NMR techniques. The HPLC method was validated according to ICH guidelines for asperosaponin VI and its related impurities.
Seven related impurities (Imp 1-7) were isolated from asperosaponin VI bulk drug. Impurity 3 was found to be a mixture of two epimers, and was first reported in the paper. The validation results showed good sensitivity, specificity, linearity (r(2) ≥ 0.997 9), precision (RSD < 5.0%), accuracy (recoveries in the range of 94.61%-106.51%) and robustness.
The developed HPLC method is suitable for the quality control of asperosaponin VI bulk drug.
研究重楼皂苷 VI 原料药中的有关物质，并建立高效液相色谱法（HPLC）测定重楼皂苷 VI 及其有关物质的方法。
采用 ODS 柱层析和半制备 HPLC 方法，从重楼皂苷 VI 原料药中检测到相关杂质，通过 TOF-MS、IR、NMR 等技术对其结构进行了阐明。按照 ICH 指南对重楼皂苷 VI 及其有关物质进行了 HPLC 方法验证。
从重楼皂苷 VI 原料药中分离得到 7 种有关物质（Imp1-7）。杂质 3 被发现是两个差向异构体的混合物，这在文献中尚属首次报道。验证结果表明，该方法灵敏度高、专属性强、线性关系良好（r²≥0.9979）、精密度（RSD<5.0%）、准确度（回收率在 94.61%-106.51%范围内）和稳健性良好。
所建立的 HPLC 方法适用于重楼皂苷 VI 原料药的质量控制。
