液相色谱-串联质谱法分析丹酚酸A的相关物质

目的研究丹酚酸A原料药中的微量杂质,并推测其可能的结构。方法采用液相色谱质谱联用技术获取微量杂质的分子量和碎片信息,并结合其紫外光谱来对未知化合物进行定性。色谱柱为Aglient XB-C18(250mm×5mm,5μm),乙腈-0.2%乙酸水二元梯度洗脱,流速1.0mL.min-1,DAD检测;质谱仪为LCQ Advantage,负离子,一至二级全扫描。结果通过液质联用分析共检测到3个含量在0.1%以上的杂质。结论根据其准分子离子和碎片信息,推测其中两个为丹酚酸A双键顺反异构化的产物,另一个为丹酚酸C。

Study on the related substances of Salvianolic acid A by HPLC-MS/MS

OBJECTIVE Our aim of this study was to analyze and deduce the structures of some trace substances in Salvianolic acid A material.METHODS A method employing on-line high performance liquid chromatography coupled with tandem mass spectrometry was selected to obtain their pseudo-molecule ions and characteristic fragments.Further,their UV spectra will give more structural information.Chromatographic analysis was performed on an Aglient XB-C18(250mm×5mm,5μm) column eluted by a mixed mobile-phase of acetonitrile and 0.2% acetic acid in water at 1.0mL·min-1.A DAD and a mass spectrometer(LCQ Advantage) were coupled with this column as detectors.The MS instrument was operated in negative mode.Then full scan and MS2 analyses were employed to gain the abundant structure information of Salvianolic acid A and its related substances.RESULTS Three trace compounds whose content was more than 0.1% were registered.CONCLUSION Based on their MS/MS and UV data,two of them were preferred to be cis-trans isomers of Salvianolic acid A.And the third compound was tentatively identified as Salvianolic acid C.