Safety Monitoring

Study on correlation between impurity profile and production process of daidzein

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  • 1. Beijing Institute For Drug Control,NMPA Key Laboratory for Research and Evaluation of Generic Drugs,Beijing Key Laboratory of Analysis and Evaluation on Chinese Medicine, Beijing 102206, China;
    2. Shanxi Province Inspection and Testing Center, Taiyuan 030031, China

Revised date: 2022-12-30

  Online published: 2024-06-24

Abstract

Objective: To study the impurity profiling of Daidzein and its correlation with production process.Methods: Impurities were quantitatively detected by HPLC with a C18 column (250 mm×4.6 mm, 5 μm). Mobile phase was water-acetonitrile (65∶35) and detection wavelength was 249 nm. The flow rate was 1.0 mL·min-1, column temperature was 30 ℃ and the injection volume was 20 μL. The run time was 6 times of Daidzein retention time. The impurity structure was confirmed via liquid chromatography-ion trap mass spectrometry analysis (MS1 and MS2) and NMR analysis (1H-NMR spectrum and 13C-NMR spectrum).Impurity source was proposed by the study of production process. Corresponding advice for process improvement was listed according to the analysis of impurity formation.Results: The main impurity in Daidzein bulk drug and pharmaceutical products was impurity A which was mainly introduced in synthesis process of bulk drug. Impurity A was related to N, N-dimethylformamide dimethyl acetal and ethanol used in process. Conclusion: This paper mainly studies detection of daidzein impurity via HPLC and structure confirmation of main impurity by NMR. Fragmentation behavior of isoflavones in mass spectrometry is elucidated. It is of great importance for process improvement, quality standard revision and daidzein derivatives synthesis.

Cite this article

SHAO Peng, ZHANG Zhe, ZHANG Ying, LIU Jian-zhen, HU Qin . Study on correlation between impurity profile and production process of daidzein[J]. Chinese Journal of Pharmaceutical Analysis, 2023 , 43(2) : 334 -340 . DOI: 10.16155/j.0254-1793.2023.02.17

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