摘要
目的:建立HPLC-ESI/TOF-MS法分析穿琥宁注射液中未知降解产物。方法:采用Inertsil ODS-3色谱柱,以甲醇-0.2%甲酸溶液为流动相;质谱检测器采用ESI离子源,在正、负离子模式下采集数据,分析降解产物结构信息。结果:发现穿琥宁注射液中有2个主要降解产物且互为同分异构体,并通过色谱分离得到相应的单体化合物,最后根据电喷雾质谱正、负离子模式下得到的准分子离子峰信息,并结合红外光谱、核磁共振谱等波谱方法鉴定这2个降解产物分别为14-脱羟-11,12-二脱氢穿心莲内酯-3-琥珀酸单酯和14-脱羟-11,12-二脱氢穿心莲内酯-19-琥珀酸单酯。结论:本法可以检测出穿琥宁注射液中的2个主要降解产物。
Objective：To establish a high performance liquid chromatography with electrospray ionization and qua- drupole - time of flight tandem mass spectrometry （ HPLC - ESI/TOF - MS） method for the analysis of unknown degradation products in potassium dehydroandrographolide succinate injection. Method：Degradation products were isolated on Inertsil ODS -3 columns with mobile phase of methanol -0. 2% formic acid and detected at 251 nm. Electrospray ionization（ESI） source was used at both positive and negative models. Results ：Two compounds, 14 - deoxy - 11,12 - didehydroandro grapholide - 3 - succinate monoester and 14 - deoxy - 11,12 - didehydroandrogra- pholide - 19 - succinate monoester, were respectively identified on the basis of quasi - molecular ion peaks by HPLC - ESI/TOF - MS, along with spectroscopic methods. Conclusion： This method can be used to determine the two major degradation products in potassium dehydroandrogapholide succinate injection.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2013年第3期454-457,485,共5页
Chinese Journal of Pharmaceutical Analysis
