超高效液相色谱-质谱联用法分析黄藤素及其主要杂质

摘要

目的 采用超高效液相色谱-质谱法(UPLC-ESI-MS)分析黄藤素中的有效成分及其主要杂质并对其结构进行确证.方法 色谱柱为ACQUITY UPLC BEH C18(2.1 mm×50 mm,1.7 μm),流动相为乙腈-0.1％甲酸水溶液(15:85)；离子源:ESI离子源；扫描模式:正离子扫描.结果 通过串联三重四极杆一级、二级质谱图的分析对黄藤素的结构进行了确证并推断出了2个主要杂质的结构.结论 检测结果对黄藤素原料药的结构确证、杂质分析、质量控制和制备工艺的改进具有重要作用.%Objective To establish an UPLC-ESI-MS method for the identification of fibriuretinin and major impurities.Methods The UPLC was performed on a ACQUITY UPLC BEHC 18 column (2.1 mm × 50 mm,1.7 μm)with acetonitrile-0.1％ formic acid aqueous solution (15∶85)as mobile phase.Data was collected under positive ion modes with ESI ion source.Results The chemical structures of fibriuretinin and two impurities were elucidated.Conclusion The results of determination offer the scientific data for studying the origin of fibriuretinin and the impurities and improving its quality.