石杉碱甲注射液金属离子诱导降解杂质结构分析

叶高兵,何佳佳,李煜,郑国钢,*

中国药学杂志 ›› 2015, Vol. 50 ›› Issue (7) : 634-638.

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中国药学杂志
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中国药学杂志 ›› 2015, Vol. 50 ›› Issue (7) : 634-638. DOI: 10.11669/cpj.2015.07.015
论著

石杉碱甲注射液金属离子诱导降解杂质结构分析

  • 叶高兵1,何佳佳2,李煜2,郑国钢1,2*
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Identification of a Metal Ion-Induced Degradation Impurity in Huperzine A Injection

  • YE Gao-bing1,HE Jia-jia2, LI Yu1,ZHENG Guo-gang1,2*
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摘要

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。

Abstract

OBJECTIVE To identify the structure of an impurity of huperzine A injection.METHODS HPLC-QTOF-MS was adopted to analyze the structure of the impurity, which was further isolated and prepared by prep-HPLC and the structure was established on the basis of spectroscopic data.RESULTS The impurity was elucidated as(11E)-7,8-dichloro-5-amino-11-ethylidene-7-methyl-5,8,9,10-tetrahydro-5,9-methenecyclooctatriene pyridin-2(1H)-one.CONCLUSION The impurity was deduced as a metal ion-induced degradation product. This investigation provides reference for the improvement of quality control and process optimization of huperzine A injection.

关键词

石杉碱甲注射液 / 杂质Ⅰ / 液质联用 / 制备高效液相色谱法 / 核磁共振

Key words

huperzine A injection / impurity Ⅰ / HPLC-MS / prep-HPLC / NMR

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叶高兵,何佳佳,李煜,郑国钢,*. 石杉碱甲注射液金属离子诱导降解杂质结构分析[J]. 中国药学杂志, 2015, 50(7): 634-638 https://doi.org/10.11669/cpj.2015.07.015
YE Gao-bing,HE Jia-jia, LI Yu,ZHENG Guo-gang,*. Identification of a Metal Ion-Induced Degradation Impurity in Huperzine A Injection[J]. Chinese Pharmaceutical Journal, 2015, 50(7): 634-638 https://doi.org/10.11669/cpj.2015.07.015
中图分类号： R927   

参考文献

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