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

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。     

HPLC-UV-ESI-MSn法分离鉴定葛根素原料药中4种有关物质

A rapid, accurate and simple HPLC-UV-ESI-MSⁿ method was developed for the separation and characterization of related impurities in puerarin bulk drug. The molecular structures and mechanism for the fragmentations of the related impurities were proposed by the MSⁿ results obtained, and confirmed by ESI-FTICR-MS which provided accurate molecular formulations at high mass resolution. The molecular structures of the four related impurities are identified as 3’-hydoxypuerarin, genistin-8-C-glucoside, neopuerarin B and neopuerarin A on the basis of fragmentation mechanism and reference data.