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

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

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.

Keywords: HPLC-UV; Method validation; Related impurities; Structure characterization; asperosaponin VI.

Publication types

  • Evaluation Study
  • Research Support, Non-U.S. Gov't

MeSH terms

  • Chromatography, High Pressure Liquid / methods*
  • Drug Contamination / prevention & control*
  • Magnetic Resonance Spectroscopy
  • Mass Spectrometry
  • Molecular Structure
  • Saponins / chemistry*

Substances

  • Saponins
  • akebia saponin D