阿洛西林钠有关物质测定方法的改进  

Improvement on the determination method of related substances in azlocillin sodium

作　　者：吴静萍 郑挺 高丹玲 WU Jingping;ZHENG Ting;GAO Danling(Fujian Institute for Food and Drug Quality Control,Fuzhou 350001,China)

机构地区：[1]福建省食品药品质量检验研究院,福州350001

出　　处：《中国药品标准》2021年第5期487-492,共6页Drug Standards of China

摘　　要：目的:改进阿洛西林钠现行标准中有关物质的测定方法。方法:采用高效液相色谱法,用十八烷基硅烷键合硅胶为填充剂,以磷酸盐缓冲液-乙腈(85∶15)为流动相A,以磷酸盐缓冲液-乙腈(70∶30)为流动相B,梯度洗脱;流速1.0 mL·min^(-1),检测波长210 nm,柱温40℃,进样体积20μL;采用主成分自身对照法计算有关物质含量。结果:阿洛西林峰与各有关物质峰分离良好,阿洛西林在0.1~100μg·mL^(-1)范围内线性关系良好,检出限为0.4 ng,精密度与重复性均符合规定。结合样品考察,优化后的方法所测得的杂质总量及杂质个数较现行方法有显著增加。结论:优化后的有关物质检测方法的分离效能优于现行标准方法,能更真实地反映产品杂质情况、更有效地控制产品的质量。Objective:To optimize the method for determination of related substances in azlocillin sodium.Methods:The test was performed in C_(18) column under the gradient elution of phosphate buffer solution-acetonitrile(85∶15)as mobile phase A and phosphate buffer solution-acetonitrile(70∶30)as mobile B.The flow rate was 1.0 mL·min^(-1),the column temperature was 40℃,the detection wavelength was 210nm and the injection volume was 20μL.The contents of related substances were calculated by principle component self control method.Results:The peaks of Azlocillin and its related substances was separated well.The linear range of azlocillin fell into 0.1^(-1)00μg·mL^(-1),and the limit of detection was 0.4 ng.There were the good precision and repeatability test results.The test results of samples showed that the optimized method determined the higher content of total impurity and more impurities.Conclusion:The optimized method of related substances has better separation performance than compendial method.It can determine the impurities accurately and,be used to control the quality of azlocillin sodium effectively.

关 键 词：阿洛西林钠 有关物质 高效液相色谱法 方法优化 质量控制 

分 类 号：R921.2[医药卫生—药学]