注射用盐酸头孢吡肟降解杂质研究

周向荣; 李硕; 汤林熹; 赖振洪; 康圆; 曾环想; 钟佳胜

doi:10.13748/j.cnki.issn1007-7693.20240784

注射用盐酸头孢吡肟降解杂质研究

Analysis of Degradation Impurities in Cefepime Hydrochloride for Injection

摘要

摘要:
目的建立高效液相色谱-四级杆-飞行时间质谱(HPLC-Q-TOF/MS)方法，对注射用盐酸头孢吡肟的降解杂质谱进行系统分析。
方法采用Inertsil ODS-3 (4.6 mm×250 mm，5 μm)色谱柱，以0.1%甲酸-水溶液(用氨水调节pH值至5.0)和乙腈为流动相梯度洗脱，流速为1.0 mL∙min⁻¹。采用电喷雾离子源ESI，正离子检测模式，通过一级和二级质谱信息对杂质进行结构解析。
结果所建立的分析方法可有效分离注射用盐酸头孢吡肟的降解杂质，通过HPLC-Q-TOF/MS鉴定出8个主要降解产物的结构，推测了头孢吡肟的降解途径。
结论本方法可用于注射用盐酸头孢吡肟的杂质研究，同时，研究结果为注射用盐酸头孢吡肟的生产运输贮藏、全面质量控制和临床应用提供了参考。

Abstract:
OBJECTIVE To establish a high performance liquid chromatography-quadrupole-time of flight mass spectrometry(HPLC-Q-TOF/MS) method for the analysis of degradation impurities in cefepime hydrochloride for injection.
METHODS Chromatographic separation was performed on an Inertsil ODS-3 column (4.6 mm×250 mm, 5 μm) with 0.1% formic acid-water solution (adjust pH to 5.0 with ammonia solution) and acetonitrile as mobile phase by gradient elution at a flow rate of 1.0 mL∙min⁻¹. The structure of impurities was identified by MS and MS/MS information obtained using an electrospray ionization (ESI) source in positive ion mode.
RESULTS The established method could effectively separate impurities in cefepime hydrochloride for injection. Eight major degradation impurities in drug were identified, and degradation pathways of cefepime was proposed.
CONCLUSION The HPLC-Q-TOF/MS method can be used to analyze impurities in cefepime hydrochloride for injection, and the results can provide reference for manufacture, transport, storage, quality control and clinical use of cefepime hydrochloride for injection.

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