液相色谱-质谱联用技术鉴定奥美沙坦酯有关物质

Identification of related substances in olmesartan medoxomil by LC-MS/MS

目的:采用液相色谱-质谱联用技术对奥美沙坦酯中有关物质进行结构鉴定。方法:采用LiChrospher C8(250 mm×4.6 mm,5μm)色谱柱,以甲醇-醋酸铵缓冲液为流动相梯度洗脱,对奥美沙坦酯有关物质进行分离;采用LC-MS/MS电喷雾正离子化测定各有关物质的相对分子质量和二级质谱,并进行结构解析。结果:检测到奥美沙坦酯粗品中11个有关物质,并推测出它们的化学结构均为奥美沙坦母核结构未发生变化的不同取代咪唑和四氮唑联苯衍生物。结论:色谱-质谱联用技术能够有效地用于药物中有关物质的鉴定,奥美沙坦酯有关物质研究可为其质量控制和工艺优化提供参考依据。

Objective：To use hyphenated techniques for the identification of related substances in olmesartan medoxomil. Methods： An LC -MS/MS method was established by using a LiChrospher C8 （250 mm × 4.6 mm,5 μm） column with gradient elution by a mobile phase consisting of methanol and ammonium acetate buffer solution. Electrospray ionization （ESI） source was operated in positive ion mode. The parent ions and the product ions of the related substances were acquired and elucidated. Results： Eleven related substances were found in olmesartan medoxomil raw material and their structures were elucidated as the different substituents having the same frame structure as olmesartan medoxomil. Conclusion：The hyphenated LC - MS method is useful for the investigation of related substances in pharmaceuticals. The related substances found in olmesartan medoxomil are valuable for its manufacturing process and quality control.