目的 快速鑒定阿莫西林原料藥中的有關(guān)物質(zhì)。方法 采用UPLC-TOF-MS/MS法測(cè)定。Waters Acquity UPLC^TM BEH色譜柱(100 mm×2.1 mm, 1.7 μm);流動(dòng)相為乙酸銨體系;體積流量0.5 mL/min;檢測(cè)波長(zhǎng)254 nm;柱溫30 ℃;進(jìn)樣量10 μL。電噴霧電離源;正離子檢測(cè);毛細(xì)管電壓3.0 kV;離子源溫度120 ℃;霧化氣溫度500 ℃;霧化氣體積流量700 L/h;錐孔氣體積流量50 L/h。結(jié)果 推測(cè)了阿莫西林原料藥中6個(gè)雜質(zhì)的化學(xué)結(jié)構(gòu)及其裂解規(guī)律, 同時(shí)與歐洲藥典中的雜質(zhì)進(jìn)行了比對(duì)歸屬。結(jié)論 建立的UPLC-TOF-MS/MS的方法和實(shí)驗(yàn)數(shù)據(jù)可為阿莫西林原料藥的質(zhì)量控制提供了重要依據(jù)。

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 UPLC^TM 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 kV, 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.

國(guó)家重大新藥創(chuàng)制項(xiàng)目(2009ZX09313-026)