注射用头孢西丁钠有关物质测定方法的改进  

Improvement on the HPLC method for determination of related substances in cefoxitin sodium for injection

作　　者：王强 韩彬 王韵 杨天风 李聪颖 高燕霞 Wang Qiang;Han Bin;Wang Yun;Yang Tianfeng;Li Congying;Gao Yanxia(Hebei Institute for Drug and Medical Device Control,Shijiazhuang 050020;Hebei University of Science and Technology,Shijiazhuang 050018)

机构地区：[1]河北省药品医疗器械检验研究院,石家庄050020 [2]河北科技大学,石家庄050018

出　　处：《中国抗生素杂志》2024年第3期341-347,共7页Chinese Journal of Antibiotics

摘　　要：目的改进注射用头孢西丁钠有关物质的测定方法。方法采用苯基硅烷键合硅胶为填充剂(Inertsil Ph-3色谱柱4.6 mm×250 mm,3μm);以甲酸铵缓冲液(取甲酸铵1.0 g,加水1000 mL使溶解,用甲酸调节pH值至2.7)为流动相A,乙腈为流动相B,按线性梯度洗脱,流速为1.0 mL/min,柱温为35℃,检测波长为254 nm。结果头孢西丁峰与各杂质峰分离良好,头孢西丁在0.0446~13.3692μg/mL范围内线性良好,检出限为0.89 ng,精密度与重复性均符合规定。结论本方法灵敏度高,分离效果好,可现实对头孢西丁钠已知杂质和聚合物杂质进行同时检测。Objective This study improved the determination method of related substances in cefoxitin sodium for injection.Methods The column of phenyl silane-bonded silica gel as filler(Inertsil Ph-3,4.6 mm×250 mm,3μm)was used,and the mobile phase was composed of mobile phase A(1.0 g/L solution of ammonium formate adjusted to pH 2.7 with formic acid)and mobile phase B(acetonitrile)to carry out gradient elution.The flow rate was 1.0 mL/min.The column temperature was 35℃and the detection wavelength was 254 nm.Results The peaks of cefoxitin sodium and its related substances were separated well.The linearity was good within the range of 0.0446~13.3692μg/mL,and the limit of detection was 0.89 ng.Precision and repeatability met the requirements.Conclusion The method had the advantages of high sensitivity and good resolution,and could be used for the simultaneous detection of impurities and polymers.

关 键 词：注射用头孢西丁钠 有关物质 聚合物 方法优化 质量控制 

分 类 号：R978.1[医药卫生—药品]