HPLC法测定注射用头孢呋辛钠有关物质方法的优化

Method Optimization of Related Substances in Cefuroxime Sodium for Injection by HPLC

目的:根据一致性评价要求提升注射用头孢呋辛钠中有关物质方法,证明该方法能将潜在的有机杂质检测出来,更好地控制药品的安全性。方法:采用高效液相色谱法。色谱柱采用Agilent Zorbax SB-C8,流动相A、B分别为醋酸盐缓冲液(取醋酸钠0.68g,冰醋酸5.8g,加水稀释至1000mL,用冰醋酸调节pH值至3.4)和乙腈(梯度洗脱),流速为1.5mL/min;检测波长为:273nm;柱温为:25℃;进样量为20μL。结果:在该色谱条件下,头孢呋辛、11个已知杂质(杂质A、B、C、E、F、G、H、I、8、9、11)分离度均大于1.5。在考察的浓度范围内,线性关系良好(r≥0.9999);平均回收率为98.75%~109.1%(RSD为1.29%~4.81%);各杂质定量限浓度远低于控制限度。结论:该方法专属性强、准确度高,可用于注射用头孢呋辛钠有关物质的测定。

Objective:According to the consistency evaluation requirements,improve the related substances method in cefuroxime sodium for injection,proving that the method can detect potential organic impurities and better control the safety of the drug.Methods:HPLC method was adopted.The determination was performed on Agilent Zorbax SB-C8 column with mobile phase a consisted of acetate buffer(0.68 g of sodium acetate,5.8 g of glacial acetic acid,dilute to 1000 mL and adjust pH to 3.4 with glacial acetic acid)and acetonitrile(gradient elution)at the flow rate of 1.5 mL/min.The detection wavelength was set at 273 nm.The column temperature was 25℃.The sample size was 20μL.Results:Under this chromatographic conditions,the resolutions of cefuroxime and 11 known impurities(impurities A,B,C,E,F,G,H,I,8,9,11)were more than 1.5,within the measured concentration range,the linear relationships were good(r≥0.9999).Average recoveries were 98.75%~109.1%(RSD were 1.29%~4.81%);The limits of quantitation of each impurity were far lower than controled limits.Conclusion:This method is specific and accurate,and can be used for the determination of related substances in cefuroxime sodium for injection.