液-质联用技术鉴定安立生坦有关物质
Identification of related substances in ambrisentan by LC-MS/MS
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摘要: 采用液相色谱-飞行时间质谱(LC-TOF/MS)和液相色谱-二级质谱联用(LC-MS/MS)两种液-质联用技术对安立生坦有关物质进行结构鉴定。采用XBridge C18(4.6 mm×150 mm，3.5 μm)色谱柱，以乙腈-水溶液(含0.15%甲酸)为流动相线性梯度洗脱，对安立生坦及其有关物质进行分离；通过电喷雾正离子化TOF/MS检测，并结合MS/MS碎片和对照品对照鉴定各有关物质的结构。在建立的色谱条件下安立生坦及其有关物质均分离良好，共检测到10个有关物质，并通过联用技术和有机反应机制解析确证了它们的结构。液-质联用技术能够有效地鉴定安立生坦有关物质，为其质量控制和工艺优化提供参考依据。Abstract: An LC-TOF/MS and LC-MS/MS method was established for the identification the related substances in ambrisentan. HPLC separation was carried out on an XBridge C18 column(4. 6 mm×150 mm, 3. 5 μm)with linear gradient elution using a mobile phase consisting of acetonitrile, water and 0. 15% formic acid. The structures of the related substances were identified by electrospray positive ESI high resolution TOF/MS and MS/MS spectra, and verified further through reference substances. Ambrisentan and its related substances can be separated with the established HPLC conditions. Ten related substances were detected and identified. The established method is useful for the identification of related substances in ambrisentan. The results obtained are valuable for its manufacturing process optimization and quality control.
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Keywords:
- ambrisentan /
- related substances /
- LC-TOF/MS /
- LC-MS/MS
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