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

关键词:  头孢哌酮钠舒巴坦钠  高分子聚合物  分子排阻色谱法

Key words:  cefoperazone sodium and sulbactam sodium  high molecular polymers  molecular exclusion chromatography

摘要:

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(15.0 mm×300 mm)，以pH 7.0的0.05 mol·L^-1磷酸盐缓冲液[0.05 mol·L^-1磷酸氢二钠溶液-0.05 mol·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5.01~250.71 μg·mL^-1(r=0.999 9)；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=0.999 9)；定量限为0.14 μg；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。

Abstract:

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.