【作者】 陈月琴； 宋敏； 杭太俊；

【Author】 CHEN Yue-qina,SONG Mina,HANG Tai-jun a (Department of Pharmaceutical Analysis,Nanjing 210009,China)

【机构】 中国药科大学药物分析教研室；

【摘要】 目的:采用色谱-质谱联用技术对盐酸法舒地尔的有关物质进行结构鉴定。方法 :采用WondaSil C18(250mm×4.6mm,5μm)色谱柱,甲醇-醋酸铵缓冲溶液(1L中含有醋酸2.0ml和醋酸铵2.0g)流动相梯度洗脱,对盐酸法舒地尔有关物质进行分离;采用LC-TOF/MS测定各有关物质的精密质量,LC-MS/MS测定二级质谱并进行结构解析。结果 :在所建立的条件下,盐酸法舒地尔及其有关物质分离良好,检测出3个有关物质,并通过联用技术和有机反应机制鉴定结构。结论 :色谱-质谱联用技术能有效地鉴定盐酸法舒地尔有关物质,为其质量控制和工艺优化提供了参考依据。更多还原

【Abstract】 OBJECTIVE:To identify the related substances in Fasudil Hydrochloride by hyphenated techniques.METHODS:A WondaSil C18 (250mm×4.6mm,5μm) column was used with a mixture of methanol and ammonium acetate buffer solution as the mobile phase with gradient elution.The related substances were identified by LC-TOF/MS and LC-MS/MS.RESULTS : Fasudil Hydrochloride and the related substances were separated under the established HPLC condition.Three related substances in Fasudil Hydrochloride were characterized by hyphenated techniques as well as organic reaction mechanism.CONCLUSION: The hyphenated LC-MS method is useful for the identification of related substances in pharmaceuticals.Identification of the related compounds in Fasudil Hydrochloride is valuable for its manufacturing process optimization and quality control.更多还原