| 高效液相色谱/电喷雾-离子阱-飞行时间质谱法鉴定地高辛中的微量有关物质 |
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| 引用本文： | 马康,苏福海,董静,赵敏,姚巍. 高效液相色谱/电喷雾-离子阱-飞行时间质谱法鉴定地高辛中的微量有关物质[J]. 中国药学杂志, 2012, 47(8): 608-612 |
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| 作者姓名： | 马康 苏福海 董静 赵敏 姚巍 |
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| 作者单位： | 中国计量科学研究院分析科学与化学计量研究所;岛津国际贸易公司北京分析中心 |
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| 基金项目： | 国家质检总局食品安全专项(ASPAQ1010);中国计量科学研究院基础科研费(AJDYX1116) |
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| 摘 要： | 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。
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| 关 键 词： | 地高辛 异羟基洋地黄毒苷 高效液相色谱/电喷雾-离子阱-飞行时间质谱 异羟基洋地黄毒苷元双洋地黄毒糖单葡萄糖苷 异羟基洋地黄毒苷元洋地黄毒糖单葡萄糖苷
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| 收稿时间： | 2000-01-01; |
Identification of Trace Impurities in Digoxin by High Performance Liquid Chromatography/Electrospray Ionization Ion Trap Time-of-Flight Mass Spectrometry |
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| MA Kang,SU Fu-hai,DONG Jing,ZHAO Min,YAO Wei. Identification of Trace Impurities in Digoxin by High Performance Liquid Chromatography/Electrospray Ionization Ion Trap Time-of-Flight Mass Spectrometry[J]. Chinese Pharmaceutical Journal, 2012, 47(8): 608-612 |
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| Authors: | MA Kang SU Fu-hai DONG Jing ZHAO Min YAO Wei |
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| Affiliation: | 1.Division of Chemical Metrology and Analytical Science,National Institute of Metrology of China,Beijing 100013,China;2.Shimadzu International Trade Ltd(Shanghai),Analytical Applications Center,Beijing 100020,China) |
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| Abstract: | OBJECTIVE To establish a rapid and accurate high performance liquid chromatography/mass spectrometry method for the analysis of impurities in digoxin crude drug.METHODS An HPLC-ESI-IT-TOF method was established.The fragmentation pathways of digoxin and digitoxin standards were studied.RESULTS A total of 12 impurities were identified or tentatively characterized based on the fragmentation pathway.Digoxigenine-bisdigitoxoside-mono-glucose digoxigenin-tridigitoxosido-monoglucose were found for the first time in digoxin.CONCLUSION It is extremely simple using HPLC-ESI-IT-TOF to provide chemical information concerning the constituents in Chinese herbal medicines,and it makes the identification results more convinced.The method has been applied for the international comparison study and given good results. |
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| Keywords: | digoxin digoxigenin high performance liquid chromatography / electrospray achieve ionization ion trap-time-of-flight mass spectrometry digoxigenine-bisdigitoxoside-mono-glucose digoxigenin-tridigitoxosido-monoglucose |
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