Isolation, structure characterization and quantification of related impurities in asperosaponin VI.
10.1016/S1875-5364(13)60063-1
- Author:
De JI
1
;
Yun-Fei LIU
;
Qiao-Han WANG
;
Chun-Feng ZHANG
;
Zhong-Lin YANG
Author Information
1. State Key Laboratory of Natural Products and Functions, China Pharmaceutical University, Nanjing 210009, China.
- Publication Type:Journal Article
- Keywords:
HPLC-UV;
Method validation;
Related impurities;
Structure characterization;
asperosaponin VI
- MeSH:
Chromatography, High Pressure Liquid;
methods;
Drug Contamination;
prevention & control;
Magnetic Resonance Spectroscopy;
Mass Spectrometry;
Molecular Structure;
Saponins;
chemistry
- From:
Chinese Journal of Natural Medicines (English Ed.)
2013;11(4):419-426
- CountryChina
- Language:English
-
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.
