阿莫西林原料药中有关物质的UPLC-TOF-MS/MS鉴定  

Identification of related substances in amoxicillin active pharmaceutical ingredients by UPLC-TOF-MS/MS

作　　者：雷勇胜[1] 宋丽明[1] 郝英魁[1] 王云 李瑜 蒋庆峰[1] 

机构地区：[1]天津药物研究院有限公司,天津300193 [2]沃特世科技有限公司,北京100026

出　　处：《现代药物与临床》2015年第1期24-27,共4页Drugs & Clinic

基　　金：国家重大新药创制项目(2009ZX09313-026)

摘　　要：目的快速鉴定阿莫西林原料药中的有关物质。方法采用UPLC-TOF-MS/MS法测定。Waters Acquity UPLCTM BEH色谱柱(100 mm×2.1 mm,1.7μm);流动相为乙酸铵体系;体积流量0.5 m L/min;检测波长254 nm;柱温30℃;进样量10μL。电喷雾电离源;正离子检测;毛细管电压3.0 k V;离子源温度120℃;雾化气温度500℃;雾化气体积流量700 L/h;锥孔气体积流量50 L/h。结果推测了阿莫西林原料药中6个杂质的化学结构及其裂解规律,同时与欧洲药典中的杂质进行了比对归属。结论建立的UPLC-TOF-MS/MS的方法和实验数据可为阿莫西林原料药的质量控制提供了重要依据。Objective To establish a rapid identification method for related substances in amoxicillin active pharmaceutical ingredients. Methods UPLC-TOF- MS/MS method was used. HPLC was carried out on Waters Acquity UPLCTM BEH column（100 mm × 2.1 mm, 1.7 μm） with ammonium acetate solution as mobile phase. The detection wavelength was 254 nm and injection volume was 10 μL at the flow rate of 0.5 mL/min. The column temperature was set for 30 ℃. MS conditions were that a mass spectrometry equipped with electrospray ionization（ESI）（＋） source for detection. Capillary voltage was 3.0 k V, and source temperature was 120 ℃. The desolvation temperature and flow rate of desolvation gas were 500 ℃ and 700 L/h. The flow rate of cone gas was 50 L/h. Results The structures and fragmentation regularities of six related substances in amoxicillin were elucidated according to their MS characteristics. At the same time, related substances were compared to the impurities from European Pharmacopoeia. Conclusion UPLC-TOF-MS/MS method and results can establish a basis for quality control and stability study of amoxicillin active pharmaceutical ingredients.

关 键 词：阿莫西林 有关物质 UPLC-TOF-MS/MS 裂解规律 

分 类 号：R927.2[医药卫生—药学]