【摘要】 目的建立高效分子排阻色谱法(HPSEC)对比阿培南中的聚合物杂质进行分离分析,并采用液—质(LC-MS)联用的方法确定其分子量,进行初步研究。方法采用Protein-Park TM 60(7.8mm×300mm,10μm)色谱柱,流动相为5mmol/L的乙酸铵溶液,流速为0.5m L/min,检测波长为220nm,进样量为20μL。用LC-MS法测定聚合物杂质分子量。结果采用HPSEC法,比阿培南聚合物杂质与比阿培南能完全分离,聚合物杂质在含比阿培南0.06~0.16mg/m L浓度范围内线性关系良好(r=0.9991),重复性较好(RSD=1.6%,n=6)。采用LC-MS法推断聚合物杂质主要是比阿培南的二聚物和三聚物。结论 HPSEC法简便、灵敏、重复性好,适用于比阿培南中聚合物杂质的测定。更多还原

【Abstract】 Objective To establish the high performance size exclusion chromatography(HPSEC) method for the separation and analysis of polymerized impurities in biapenem. And the LC-MS method was used to confirm the molecule weight of the separated polymerized impurities. Methods The column was Protein-Park TM 60 Waters(7.8mm×300mm, 10μm). The mobile phase was 5mmol/L ammonium acetate solution at a flow rate of 0.5m L/min. The wavelength of UV detector was set at 220 nm. The volume of injection was 20μL. Then the LC-MS was used to confirm the molecule weight of the separated polymers in biapenem. Results The polymerized impurities in biapenem could be well separated with biapenem using HPSEC. The linear range of the polymerized impurities was 0.06~0.16mg/m L(r=0.9991), and the repeatability was fine(RSD=1.6%, n=6). The LC-MS results shown that the main polymerized impurities were dimer and trimer. Conclusion The HPSEC method was simple, accurate and sensitive for the control of the polymer in biapenem.更多还原