摘要
目的建立注射用头孢哌酮钠/舒巴坦钠中聚合物杂质的反相高效液相色谱测定法。方法以十八烷基硅烷键合硅胶为填充剂(Waters XBridge C_(18),4.6 mm×150 mm,5μm),以6.8 g/L磷酸二氢钾溶液(用磷酸调pH至3.0)-乙腈为流动相,梯度洗脱,流速为1.0 mL/min,检测波长为220 nm;柱温为28℃;进样量为20μL。结果头孢哌酮双母核杂质定量限为0.2930μg/mL(相当于供试品浓度的0.015%),检测限为0.1465μg/mL(相当于供试品浓度的0.0073%);头孢哌酮二聚体杂质B定量限为0.2979μg/mL(相当于供试品浓度的0.015%),头孢哌酮二聚体杂质B检测限为0.1490μg/mL(相当于供试品浓度的0.0073%)。在0.2930~24.4130μg/mL浓度范围内,头孢哌酮双母核杂质的线性方程为y=0.6404x-0.0184,r=1.0000。在0.2979~24.8226μg/mL浓度范围内,头孢哌酮二聚体杂质B的线性方程为y=0.5234x+0.0185,r=1.0000。头孢哌酮双母核杂质的回收率范围为90.53%~102.80%(RSD<10.0%,n=9);头孢哌酮二聚体杂质B的回收率范围为91.35%~100.25%(RSD<10.0%,n=9)。结论该方法简便,专属性好,准确度高,灵敏度好,可有效测定头孢哌酮钠/舒巴坦钠中的聚合物杂质。
Objective To establish a reverse high-performance liquid chromatography(RP-HPLC)method to determine the polymer impurities in cefoperazone sodium and sulbactam sodium for injection.Methods The column with 4.6 mm×150 mm and 5μm packing octadecylsilyl silica gel(Waters XBridge C_(18))was used.6.8 g/L potassium dihydrogen phosphate solution(pH adjusted to 3.0 with phosphoric acid)-acetonitrile was utilized as the mobile phase,and the gradient elution program was the linear gradient elution at 1.0 mL/min of flow rate.The detection wavelength was 220 nm,column temperature was 28℃and injection volume was 20μL.Results The LOQ of cefoperazone double arents impurity was 0.2930μg/mL(corresponding to 0.015%of sample concentration),and the LOD was 0.1465μg/mL(corresponding to 0.0073%of sample concentration).The LOQ of cefoperazone dimer impurity B was 0.2979μg/mL(corresponding to 0.015%of sample concentration),and the LOD was 0.1490μg/mL(corresponding to 0.0073%of sample concentration).The calibration curve for cefoperazone double arents impurity was linear in the concentration range of 0.2930μg/mL to 24.4130μg/mL(y=0.6404x-0.0184,r=1.0000);the calibration curve for cefoperazone dimer impurity B was linear in the concentration range of 0.2979μg/mL to 24.8226μg/mL(y=0.5234x+0.0185,r=1.0000).The recoveries of cefoperazone double arents impurity were 90.53%to 102.80%(RSD<10.0%,n=9),and the recoveries of cefoperazone dimer impurity B were 91.35%to 100.25%(RSD<10.0%,n=9).Conclusion The technique for identifying polymer impurities in cefoperazone sodium and sulbactam sodium for injection is straightforward,specific,accurate and sensitive.
作者
刘洋
骆献丽
陈晓英
孙冬梅
LiuYang;Luo Xianli;Chen Xiaoying;Sun Dongmei(Lepu Pharmaceuticals,Inc,Zhengzhou 450000)
出处
《中国抗生素杂志》
北大核心
2025年第11期1308-1315,共8页
Chinese Journal of Antibiotics
关键词
注射用头孢哌酮钠/舒巴坦钠
聚合物
反相高效液相色谱法
头孢哌酮双母核杂质
头孢哌酮二聚体杂质B
Cefoperazone sodium and sulbactam sodium for injection
Polymer
Reverse high-performance liquid chromatography
Cefoperazone double arents impurity
Cefoperazone dimer impurity B
