Hangzhou Minsheng Pharmaceutical Co., Ltd.

Rifampicin, essential for long-term tuberculosis treatment, requires rigorous control of non-therapeutic impurities due to their potential adverse, including mutagenic effects. Reports on control strategies for genotoxic impurities in rifampicin have been limited. This study introduced an analytical method to identify potential genotoxic impurities from the synthesis of raw materials. The structure of the 25-deacetyl-23-acetyl-rifampicin genotoxic impurity was confirmed using nuclear magnetic resonance, high-resolution mass spectrometry (HRMS), and high-performance liquid chromatography (HPLC). An HPLC-HRMS method was established and validated for detecting another genotoxic impurity, 1-amino-4-methylpiperazine, adhering to the International Council on Harmonization guidelines, which include specificity, linearity, detection and quantification limits, accuracy, precision, and robustness. These developments improve the quality control strategy for genotoxic impurities in rifampicin, ensuring product safety.

A simple and sensitive LC-MS method was developed for the separation and identification of impurities of Minomustine (MIN).MIN and its impurities were separated with gradient elution LC system and detected using a hybrid quadrupole ion trap mass spectrometer.Forced degradation experiments were also performed under acid/base hydrolysis, heat, light, and oxidation conditions.Four impurities were detected in MIN bulk drug, among which the contents of three increased under the stress conditions.The structures of these impurities were elucidated based on the QTRAP MSⁿ data and further validated by accurate mass data.To the best of our knowledge, three of these impurities were identified for the first time.In addition, the ¹H and ¹³C NMR data of impurity IV were first assigned in this paper.

[Objective] The research aimed to establish the HPLC specific chromatogram of rehmannia formula granule and to determine acteoside content.[Method] For characteristic chromatograms, chromatog. experiments were performed with the mobile phase of 0.1% acetic acid-acetonitril in gradient elutione and the column temperature was set at 25°C.The detection wave length was 334 nm and the flow rate was 1.0 mL/min.[Result] The HPLC specific chromatogram of rehmannia formula granule showed 8 characteristic peaks, and the linear range of acteoside was 4.89-195.68 μg/mL (R²=0.9996), with average recovery at 101.57% (RSD=1.29%).[Conclusion] This method is simple, accurate and good reproducibility, and can provide a reference for the tech. study and quality control of rehmannia formula granule.