HPLC-UV-FTICRMS/MS^n法分离鉴定葛根素原料药中4种有关物质  

Separation and Characterization of 4 Related Impurities in Puerarin Bulk Drug by HPLC-UV-FTICRMS/MS^n

作　　者：王鹏远[1] 吴彩胜[1] 吴松[1] 张金兰[1] 

机构地区：[1]中国医学科学院北京协和医学院药物研究所,北京100050

出　　处：《质谱学报》2010年第3期143-151,共9页Journal of Chinese Mass Spectrometry Society

基　　金：卫生行业科研专项项目(200802038)资助

摘　　要：采用高效液相色谱-紫外检测器-傅里叶变换离子回旋共振质谱(HPLC-UV-FTICRMS/MSn)技术获得了葛根素及其有关物质的MSn和HRMS数据,分析其可能的裂解机制,推断有关物质的结构,并依据HRMS数据确证了有关物质及其部分碎片的分子组成,最终鉴定葛根素原料药中4种有关物质,其准分子离子峰[M+H]+分别为m/z433.112 95、433.112 92、417.118 01和417.118 01,通过质谱裂解机制研究以及与文献数据的对比,推测它们的结构分别为3’-羟基葛根素、染料木素-8-C-葡萄糖苷、新葛根素B和新葛根素A。The molecular structures and mechanism for the fragmentations of the related impurities were proposed by the MSn and HRMS results obtained by high performance liquid chromatography-ultraviolet detector-fourier transform ion cyclotron resonace mass spectrometry（HPLC-UV-FTICRMS/MSn）.The molecular compositions of the related impurities and some of the fragmentations were confirmed by the HRMS datas.Four related impurities in puerarin bulk drug were separated.Their ＋ ion peaks are m/z 433.112 95,433.112 92,417.118 01 and 417.118 01,respectively.They are identified as 3＇-hydoxypuerarin,genistin-8-C-glucoside,neopuerarin B and neopuerarin A on the basis of fragmentation mechanism and reference data.

关 键 词：葛根素 电喷雾电离(ESI) 傅里叶变换离子回旋共振质谱(FTICR-MS) 结构鉴定 

分 类 号：O657.63[理学—分析化学]