asperosaponin VI 中有关杂质的分离、结构特征描述和定量分析。

Isolation, structure characterization and quantification of related impurities in asperosaponin VI.

机构信息

State Key Laboratory of Natural Products and Functions, China Pharmaceutical University, Nanjing 210009, China.

出版信息

Chin J Nat Med. 2013 Jul;11(4):419-26. doi: 10.1016/S1875-5364(13)60063-1.

DOI:10.1016/S1875-5364(13)60063-1

PMID:23845554

Abstract

AIM

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.

METHODS

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.

RESULTS

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.

CONCLUSION

The developed HPLC method is suitable for the quality control of asperosaponin VI bulk drug.

摘要

目的

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。

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。

结果

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。