甲磺酸帕珠沙星原料及注射剂中有关物质的定性研究

Qualitative Study on the Related Substances in Pazufloxacin Mesilate and Its Injections

目的:对甲磺酸帕珠沙星原料及注射剂中主要有关物质进行定性研究。方法:采用LC-PDA-MS/MS、UPLC-TOF-MS及核磁共振仪(~1H-NMR)对甲磺酸帕珠沙星原料及注射剂中主要杂质Ⅰ和Ⅱ进行结构解析与确证。结果:对甲磺酸帕珠沙星原料及注射剂中检出的2个主要杂质Ⅰ和Ⅱ进行了结构确证,并对其进行了溯源,确定其为原料药合成副产物。结论:本研究推断杂质Ⅰ和Ⅱ分别为甲磺酸帕珠沙星甲酯和甲磺酸帕珠沙星乙酯,为甲磺酸帕珠沙星原料及其注射剂工艺和质量控制提供参考。

Objective:To conduct the qualitative study on the main impurities in pazufloxacin mesilate and its injections.Methods:LC-PDA-MS/MS,UPLC-TOF-MS and^1 H-NMR methods were adopted to speculate and confirm the structures of impurityⅠamdⅡ.Results:The main impurityⅠamdⅡwere detected out in pazufloxacin mesilate and its injections,and the structures of impurityⅠandⅡwere confirmed.The source of the impurities was traced,and they were by-products from the synthesis of pazufloxacin mesilate as raw material.Conclusion:The study confirmed impurity I and II respectively was methyl pazufloxacin mesylate and ethyl pazufloxacin mesylate.The obtained results are valuable for its manufacturing process monitoring and quality control.