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目的建立快速、准确鉴别地高辛中化学成分的液相色谱-质谱联用方法。方法采用高效液相色谱/电喷雾-离子阱-飞行时间质谱(HPLC/ESI-IT-TOF/MS)对异羟基洋地黄毒苷(地高辛)和洋地黄毒苷对照品进行分析,总结了二者的多级质谱裂解规律,研究质谱碎片裂解途径,建立了地高辛原料药的液相色谱分离条件及质谱分析条件。结果依据各有关物质组分的多级质谱数据,鉴定了12个主要的有关物质,其中异羟基洋地黄毒苷元双洋地黄毒糖单葡萄糖苷和异羟基洋地黄毒苷元3≥洋地黄毒糖单葡萄糖苷为地高辛原料药中首次发现的有关物质组分。结论在原料药地高辛化学成分研究工作中,采用HPLC/ESI-IT-TOF/MS可提高原料药化学成分的分析效率并有利于新化合物的发现和鉴别,对保证原料药的质量控制有重要意义。此方法已经应用到国际比对研究中,取得良好结果。
Objective To establish a rapid and accurate method for the identification of chemical components of digoxin by liquid chromatography-mass spectrometry. Methods The digoxigenin (digoxin) and digoxigenin reference substance were analyzed by HPLC / ESI-TOF / MS, and the results were summarized The two-stage mass spectrometry cleavage rules, cleavage mass spectrometry debris pathways, the establishment of the digoxin raw material liquid chromatography separation conditions and mass spectrometry conditions. Results Based on the multi-level MS data of each related substance component, 12 major related substances were identified, of which, digoxigenin diglycidyl monoglucoside and digoxigenin 3> Antibiotic sugar monoglycoside is the first substance component found in digoxin drug substance. Conclusion The HPLC / ESI-IT-TOF / MS can improve the analytical efficiency of chemical constituents of APIs and find and identify new compounds in the study of chemical constituents of digoxin of APIs. The quality control of APIs Significance. This method has been applied to international comparison and achieved good results.