改进的HPLC法检查头孢呋辛钠中有关物质

Determination of Related Substances of Cefuroxime Sodium by an Improved HPLC Method

目的:改进用于头孢呋辛钠中有关物质检查的HPLC法。方法:色谱柱为Agilent HC-C8(250 mm×4.6mm,5μm),以醋酸盐缓冲液(取醋酸钠0.68 g和冰醋酸5.8 g,加水稀释成1 000 mL的溶液,用冰醋酸调节pH值至3.4)为流动相A,乙腈为流动相B,线性梯度洗脱,流速为1.5 mL.min-1;检测波长为273 nm;进样量为20μL。结果:头孢呋辛与相邻杂质可基线分离,其在9.950～637.1 mg.L-1的范围内线性关系良好(r=0.999 9),检测限和定量限分别为0.08和0.2 mg.L-1;方法重复性良好,所测单个最大杂质含量的RSD为1.8%(n=6),总杂质含量的RSD为1.5%(n=6);方法耐用性好,适用于不同品牌的辛烷基键合硅胶色谱柱。结论:该方法专属、准确、灵敏,优于2005年版中国药典方法。

Objective ：To improve the HPLC method for the determination of related substances of cefuroxime sodium.Methods：Agilent HC-C8,a column packed with octylsilane bonded silica gel,and acetate buffer（0.68 g sodium acetate and 5.8 g glacial acetic acid were diluted with water to 1000 mL and adjusted to pH 3.4 with glacial acetic acid） as the mobile phase A and acetontrile as mobile phase B at a flow rate of 1.5 mL ·min^-1 were used with a detection wavelength of 273 nm and an injection volume of 20 μL by linear gradient elution.Results：A good resolution of the peaks of cefuroxime and adjacent impurities was obtained.The linear range was 9.950-637.1 mg ·L-1（r=0.9999） for cefuroxime sodium.The limits of detection and quantitation for cefuroxime sodium were 0.008 and 0.2 mg ·L^-1,respectively.The method had a good reproducibility with a RSD of 1.8%（n=6） for the content of the maximum individual impurity and a RSD of 1.5%（n=6） for the total content of all impurities and showed a good ruggedness for variation of type of octylsilane columns.Conclusion：The method is specific,accurate,sensitive and superior to that in ChP2005.