高效分子排阻色谱法测定注射用盐酸头孢替安高分子杂质

摘要

目的 建立高效分子排阻色谱(HPSEC)法测定注射用盐酸头孢替安高分子杂质.方法 采用TSK-Gel2000SWXL凝胶色谱柱(7.8 mm×30 cm,5μm);流动相:0.1mol·L-1磷酸盐缓冲液[0.1 mol·L-1磷酸氢二钠-0.1mol·L-1磷酸二氢钠(61:39)];流速为0.7 mL·min-1;检测波长为254 nm;柱温为30℃;进样量为20μL,外标法定量.结果 头孢替安的线性范围为5.0～25.0 μg·mL-1;检测限与定量限分别为0.1和0.246 μg· mL-1;实验RSD为0.50％(n=6);样品溶液室温放置不稳定.结论 该方法分离效率高,专属性好,为注射用头孢替安高聚物进一步研究提供参考.%Objective To establish a high performance size esclusion chromatography (HPSEC) method for the determination of high molecular weight impurities of cefotiam hydrochloride for injection.Methods A TSK G2000 SWXL column(7.8 mm × 30 cm,5μm) was used,the mobile phase consisting of phosphate budder solution [0.1 mol·L-1 disodium hyrogen phosphate-0.1 mol·L-1 sodium dihydrogen phosphate (61:39)],the flow rate was 0.7 mL· min-1,the detection wavelength was 254 nm,the column temperature was 30 ℃,the injection volume was 20 μL,and the concentration of polymers was quantified by external standard method.Results For HPSEC method,the calibration curves were linear in the range of 5.0-25.0 μg·mL-1 for cefotiam,and the LOD and LOQ was 0.1 μg·mL-1 and 0.246 μg· mL-1,the RSD for replicate for injections of reference solution was 0.50％,the sample solution was not stable in room temperature.Conclusion The method has high separation efficiency and good specificity,which provides reference for the further study of the polymer of cefotiam hydrochloride for injection.