氢溴酸沃替西汀有关物质的色谱-质谱结构鉴定  

Identification of the related substances of vortioxetine hydrobromide by LC-MS techniques

作　　者：王璐[1] 吴骁 王叶 梁方梅 杭太俊[1] 宋敏[1] WANG Lu;WU Xiao;WANG Ye;LIANG Fang-mei;HANG Tai-jun;SONG Min(Department of Pharmaceutical Analysis,China Pharmaceutical University,Nanjing 210009,China)

机构地区：[1]中国药科大学药物分析系,江苏南京210009

出　　处：《药学学报》2018年第8期1351-1356,共6页Acta Pharmaceutica Sinica

摘　　要：为了研究氢溴酸沃替西汀原料药中的有关物质,本研究采用Phenomenex Luna Phenyl-Hexyl(150mm×4.6 mm,3μm)色谱柱,以乙腈-甲酸铵缓冲液为流动相梯度洗脱分离出6个主要有关物质,结合电喷雾-四极杆-飞行时间串联质谱法(ESI-Q-TOF/MS)测定5个有关物质的母离子及碎片离子的准确质量和元素组成,大气压化学电离飞行时间质谱法(APCI-TOF/MS)测定1个有关物质的准确分子质量,三重四级杆串联质谱(MS/MS)测定其二级碎片离子特征。在所建立的条件下,氢溴酸沃替西汀及其有关物质分离良好,首次检测并鉴定出了6个主要有关物质,为氢溴酸沃替西汀的工艺优化和质量控制提供了参考依据。The study was aimed to identify the related substances of vortioxetine hydrobromide by hyphenated techniques.The separation of the six related substances was performed on a Phenomenex Luna Phenyl-Hexyl column（150 mm × 4.6 mm,3 μm） by linear gradient elution of acetonitrile and ammonium formate solution.Electrospray and atmospheric pressure chemical ionization were interfaced respectively with high resolution Q-TOF/MS for the determination of the accurate mass and elemental composition of the parent ions of the related substances,and triple quadrupole tandem mass was employed for the product mass spectra determination.The structures of the related substances were identified through elucidation of the fragment ions.Vortioxetine hydrobromide and its related substances were adequately separated under the established HPLC conditions.Six major related substances were detected and identified for the first time.The data provides a reference for optimization of the synthetic process and quality assurance of vortioxetine hydrobromide.

关 键 词：氢溴酸沃替西汀 有关物质 结构鉴定 色谱-质谱联用 

分 类 号：R917[医药卫生—药物分析学]