分子排阻色谱法测定注射用头孢哌酮钠舒巴坦钠中的高分子聚合物

Determination of High Molecular Polymers in Cefoperazone Sodium and Sulbactam Sodium for Injection by Molecular Exclusion Chromatography

目的建立注射用头孢哌酮钠舒巴坦钠中高分子聚合物的测定方法。方法采用Sephadex G-10凝胶色谱柱(15.0mm×300mm),以pH 7.0的0.05mol.L 1磷酸盐缓冲液[0.05mol.L-1磷酸氢二钠溶液-0.05mol.L-1磷酸二氢钠溶液(61∶39)]为流动相A,以水为流动相B,流速为1.2 mL.min 1,检测波长为254 nm。结果头孢哌酮高分子聚合物与头孢哌酮药物单体能较好分离,头孢哌酮自身对照的线性范围为5.01～250.71μg.mL-1(r=0.9999);在10.13～30.24 mg.mL 1内,供试品溶液浓度与聚合物峰面积呈良好线性关系(r=0.9999);定量限为0.14μg;方法精密度良好(RSD=0.50%,n=5);样品测定重复性与重现性好(RSD=0.82%,n=5;RSD=3.4%,n=3)。结论所建方法操作简便、结果可靠,可用于注射用头孢哌酮钠舒巴坦钠中高分子聚合物的检测。

OBJECTIVE To establish a method for the determination of high molecular polymers in cefoperazone sodium and sulbactam sodium for injection.METHODS Chromatographic analysis was performed on Sephadex G-10 column(15.0 mm×300 mm),0.05 mol·L 1 phosphate buffer(pH 7.0) as the mobile phase A,and super pure water as the mobile phase B.The flow rate was 1.2 mL·min 1 and the detection wavelength was 254 nm.RESULTS High molecular polymers in cefoperazone was separated completely from cefoperazone.The linear range of cefoperazone was 5.01 250.71 μg·mL 1(r=0.999 9).The linear range of the substances examined was 10.13 30.24 mg·mL 1(r=0.999 9).The limit of quantification was 0.14 μg.The RSD for replicate injections of reference solution was 0.50%(n=5),the repetitiveness and the reproducibility were fine,the RSDs were 0.82%(n=5) and 3.4%(n=3),respectively.CONCLUSION The method is simple,rapid and reliable.It is applicable for the quality control of cefoperazone sodium and sulbactam sodium for injection.