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目的对石杉碱甲注射液的杂质Ⅰ进行结构分析。方法采用高效液相-飞行时间质谱联用(HPLC-Q-TOF)技术对杂质进行解析推断,利用制备型高效液相从石杉碱甲注射液中分离制备杂质Ⅰ,结合NMR技术进行结构确证。结果利用质谱和核磁方法鉴定了石杉碱甲注射液中杂质Ⅰ:(11E)-7,8-二氯-5-氨基-11-亚乙基-5,8,9,10-四氢-7-甲基-5,9-亚甲基环辛三烯并[b]吡啶-2(1H)-酮。结论杂质Ⅰ为金属离子诱导降解产生,为石杉碱甲注射液质量控制和工艺优化提供参考依据。
OBJECTIVE: To analyze the structure of impurity Ⅰ in huperzine A injection. Methods The impurities were analyzed by high performance liquid chromatography coupled with time-of-flight mass spectrometry (HPLC-Q-TOF), and impurity Ⅰ was separated from the huperzine A injection by preparative high performance liquid phase. The structure was confirmed by NMR . Results The mass spectrometry and nuclear magnetic resonance method were used to identify the impurities in huperzine A injection Ⅰ: (11E) -7,8-Dichloro-5-amino-11-ethylidene-5,8,9,10-tetrahydro- Methyl-5,9-methylenecyclooctyclo [b] pyridin-2 (1H) -one. Conclusion Impurity Ⅰ is induced by metal ions and provides a reference for quality control and process optimization of Huperzine A injection.