高效分子排阻色谱法分析头孢噻肟钠中的聚合物___

摘要  目的：建立高效分子排阻色谱(HPSEC)法测定头孢噻肟聚合物，与2005年版中国药典方法比较，并用LC-MS对二聚物进行初步研究。方法：采用凝胶色谱柱(TSK G2000 SW，60 cm×7.5 mm)；流动相：0.01 mol·L^-1磷酸盐缓冲液[(0.01 mol·L^-1磷酸氢二钠溶液-0.01 mol·L^-1磷酸二氢钠溶液(61∶39)，用0.1 mol·L^-1磷酸调节pH至7.0]；流速1.0 mL·min^-1；检测波长254 nm。结果：HPSEC法，头孢噻肟和二聚物的线性范围分别为2.57×10^-4~0.0205 mg·mL^-1(r=1.000)和7.39×10^-4~0.0987 mg·mL^-1(r=0.9997)；二聚物的平均回收率为99.7%(n=9)，检测限为5 ng；对照品溶液重复进样的精密度(RSD)为0.20%(n=6)，样品测定的重复性(RSD)为0.94%(n=6)。药典方法，二聚物的检测限为2 μg，对照品溶液重复进样的精密度(RSD)为0.92%(n=6)，样品测定的重复性(RSD)为5.7%(n=6)。结论：HPSEC法适于测定头孢噻肟聚合物，比药典方法专属性强，灵敏度高，重复性好，操作简便。

关键词：头孢噻肟；头孢噻肟聚合物；头孢噻肟二聚物；高效分子排阻色谱法

 

 

Abstract   Objective:To establish a high performance size exclusion chromatography(HPSEC)method for the determination of cefotaxime polymer,compare with the method in ChP 2005,and make primary study on the dimer by LC-MS.Methods:A TSK G2000 SW column(60 cm×7.5 mm) was used with the mobile phase consisting of phosphate buffer solution\[0.01 mol·L^-1 disodium hydrogen phosphate-0.01 mol·L^-1 sodium dihydrogen phosphate(61∶39),adjust to a pH of 7.0 with 0.1 mol·L^-1 phosphoric acid\] at a flow rate of 1.0 mL·min^-1,and the detection wavelength was at 254 nm.Results:For HPSEC method,the calibration curves were linear in the range of 2.57×10^-4-0.0205 mg·mL^-1 for cefotaxime(r=1.000) and 7.39×10-4-0.0987 mg·mL^-1for dimer(r=0.9997),the average recovery of dimer was 99.7%(n=9),and the detection limit of dimer was 5 ng,the RSD for replicate injections of reference solution was 0.20%(n=6),and the repeatability for 6 measurement results was 0.94%.Forthe method in ChP 2005,the detection limit of dimer was 2 μg,the RSD for replicate injections of reference solution was 0.92%(n=6),and the repeatability for 6 measurement results was 5.7%.Conclusion:The HPSECmethod is suitable for determination of cefotaxime polymer,and has better specification,sensitivity,precision and simpler procedure than the method in ChP 2005.

Key words：cefotaxime;cefotaxime polymer;cefotaxime dimer;high performance size exclusion chromatography