摘要
目的:验证柱前衍生化HPLC/UV测定环维黄杨星D有关物质的可行性。方法:环维黄杨星D同异氰酸苯酯反应后,柱前衍生化HPLC/UV测定环维黄杨星D有关物质并与HPLC/MS直接测定环维黄杨星D有关物质比较。结果:衍生化反应后,主峰与有关物质分离好,所测得的有关物质与HPLC/MS直接测定的环维黄杨星D有关物质一一对应。结论:环维黄杨星D中含分子量为386,388的杂质,每分子环维黄杨星D及有关物质均同2分子异氰酸苯酯定量反应,柱前衍生化HPLC/UV可测定环维黄杨星D有关物质,与HPLC/MS直接测定法相比,本法简单、准确。
AIM To certify the practicability of determination cyclovirobuxine D. related substances by precolumn derivatization RP-HPLC. METHODS Cyclovirobuxine D reacted with a derivative reagent ]-phenyl-isocyanate to form a ultraviolet derivative, and then was seperated by RP-HPLC. The main peak and the related substances peaks were identified by diode array detecter and MS. At the same time, cyclovirobuxine D and its related substances were analyzed by HPLC/MS directly and a comparison was made between two kinds of method. RESULTS cyclovirobuxine D can be separated from its related substances easily by derivatization method but not for HPLC/MS, and the absence of interference between the derivative peak responses of cyclovirobuxine and its related substances peak were verified by UV diode array detector and MS. Two kinds of related substances can be detected by both analytical methods,and the identity of determinated cyclovirobuxine D. related substances by above two kinds of method was also proved. CONCLUSION There exsist two kinds of related substances in cyclovirobuxine D, the molecular weights are 386 which possible chemical structure elucidated is Cycloprotobuxine D or Cyclobuxine D and 388 which may be reduction product of couple bond in Cycloprotobuxine D. The derivative method is simple and accurate. It can be used for the quality control of cyclovirobuxine D. related substances.
出处
《中国药科大学学报》
CAS
CSCD
北大核心
2002年第5期408-411,共4页
Journal of China Pharmaceutical University
