HPLC-ESI/TOF-MS法分析穿琥宁注射液中的降解产物

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 quadrupole-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-didehydroandrographolide-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.

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