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目的:采用色谱-质谱联用技术鉴定头孢妥仑匹酯的有关物质,为其工艺优化和质量控制提供参考依据。方法:采用YMC-Pack ODS-AM(150 mm×4.6 mm,5μm)色谱柱,以甲醇-乙腈-乙酸铵缓冲液为流动相,梯度洗脱,对头孢妥仑匹酯有关物质进行分离;采用电喷雾正离子化-飞行时间质谱法(ESI-TOF/MS)测定各有关物质离子的准确质量和元素组成,三重四极质谱(ESI-MS/MS)测定子离子特征。结果:在所建立的条件下,头孢妥仑匹酯及其有关物质分离良好,检测并鉴定出10个主要有关物质。结论:色谱-质谱联用技术能有效地分离鉴定头孢妥仑匹酯中的有关物质,鉴定结果为其质量控制和工艺优化提供了参考。
OBJECTIVE: To identify the related substances of cefditoren diclofenac by chromatography-mass spectrometry, and to provide a reference for the process optimization and quality control. METHODS: Cefditoren pivoxil was separated on a YMC-Pack ODS-AM column (150 mm × 4.6 mm, 5 μm) using methanol-acetonitrile-ammonium acetate as mobile phase and gradient elution. The exact mass and elemental composition of each related substance ion were determined by electrospray ionisation-time of flight mass spectrometry (ESI-TOF / MS). The triple ion mass spectrometry (ESI-MS / MS) Results: Under the established conditions, cefditoren pivoxil and its related substances were well separated and 10 major related substances were detected and identified. Conclusion: Chromatography - mass spectrometry can effectively separate and identify the related substances in cefditoren diclofenac. The identification results provide a reference for its quality control and process optimization.