多糖活化剂1-氰基,4-2甲氨基吡啶四氟硼酸盐降解产物的结构分析  

Analysis of structure of degradation product of polysaccharide activator 1-cyano-4-dimethylamino-pyridinium

作　　者：董威 袁军 李红 陈煜 刘昊智 李津 庄再成 吴克 DONG Wei;YUAN Jun;LI Hong;CHEN Yu;LIU Hao-zhi;LI Jin;CHONG Pele ChoiSing;WU Ke(Bravovax Co.,Ltd,Wuhan 430075,Hubei Province,China)

机构地区：[1]武汉博沃生物科技有限公司,湖北武汉430075 [2]华东理工大学生物工程学院,上海200237

出　　处：《中国生物制品学杂志》2021年第2期152-154,160,共4页Chinese Journal of Biologicals

基　　金：武汉东湖新技术开发区第十一批“3551光谷人才计划”(武新管[2018]47号)。

摘　　要：目的分析多糖活化剂1-氰基,4-二甲氨基吡啶四氟硼酸盐(1-cyano-4-dimethylamino-pyridinium,CDAP)降解产物的结构。方法将CDAP用重水(pH 9.0)进行过夜降解,采用紫外光谱(200~400 nm)、一维核磁氢谱(1H-NMR)和碳谱(13C-NMR)分析CDAP降解前后的结构变化,并通过外标法计算降解程度。结果 CDAP在碱性环境中过夜降解后,其产物与4-二甲氨基吡啶(4-dimethylaminopyridine,DMAP)一致,降解程度达99.5%以上。结论 CDMP降解的主要产物为DMAP,应将DMAP残留纳入基于CDAP活化的多糖-蛋白结合疫苗生产过程中质量控制指标。Objective To analyze the structure of degradation product of 1-cyano-4-dimethylamino-pyridinium(CDAP),a polysaccharide activator. Methods CDAP was degraded with heavy water overnight(pH 9. 0),of which the structural change before and after degradation was analyzed by ultraviolet spectroscopy(200 ~ 400 nm),1H-NMR and 13C-NMR,and the degradation level was calculated by external standard method. Results The structure of degradation product of CDAP under basic environment was consistent with that of mainly 4-dimethylaminopyridine(DMAP),while the degradation level was more than 99. 5%. Conclusion The degradation praduct of CDAP was mainly DMAP. The analysis of DMAP should be included into the test for residues during production of CDAP activation-based polysaccharide-protein conjugate vaccine.

关 键 词：多糖活化剂 1-氰基 4-二甲氨基吡啶四氟硼酸盐 降解 

分 类 号：O657.8[理学—分析化学]