【摘要】 目的对β-内酰胺类抗生素中聚合物杂质检测的常规凝胶色谱方法进行有效性考察,并且实现凝胶色谱法与反相高效液相系统有关物质分析方法的有效统一。方法采用在线二维柱切换技术和液质联用技术对常规凝胶色谱法的有效性进行考察,同时将凝胶色谱检出的杂质在反相液相色谱系统中进行定位及结构推断。结果常规凝胶色谱法检测的盐酸头孢替安中的聚合物杂质主要为降解物杂质及开环物杂质等,无法有效的表征致敏性聚合物杂质。结论在线柱切换技术可以有效地将凝胶色谱法的优势与指针性聚合物杂质的定位结合起来,为建立真实有效的表征聚合物杂质的研究思路奠定基础。更多还原

【Abstract】 OBJECTIVE To validate the conventional gel filtration chromatography( GFC) method for determination of the polymer impurities in β-lactam antibiotics and achieve combination of GFC and RP-HPLC system. METHODS The effectiveness of the conventional GFC method was identified by 2D-GFC × LC-TOFMS and the polymer impurities found by GFC were identified by RPHPLC. RESULTS The polymer impurities found by GFC mainly were degradation impurities and open β-lactam ring impurities,which could not effectively characterize the sensitizing polymer impurities in cefotiam hydrochloride. CONCLUSION An effective method to characterize the polymer impurities in β-lactam antibiotics may be established on the basis of online column switching technique which effectively combines the advantages of GFC and the ability of RP-HPLC to identify the special impurities.更多还原