高效液相色谱-二极管阵列检测器法在头孢噻肟钠残留基因毒性杂质检测中的应用  

Application of HPLC-DAD for Genotoxic Impurity in Cefotaxime Sodium

作　　者：张莹 薛雯 单国庆 孟龙 韩勇 孔令洋 王冉 ZHANG Ying;XUE Wen;SHAN Guo-Qing;MENG Long;HAN Yong;KONG Ling-Yang;WANG Ran(Jining Institute for Food and Drug Control,Jining 272071,China;Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing100700,China)

机构地区：[1]济宁市食品药品检验检测研究院,济宁272071 [2]中国中医科学院中药研究所,北京100700

出　　处：《中国药物经济学》2023年第5期107-110,115,共5页China Journal of Pharmaceutical Economics

基　　金：山东省市场监督管理局2021年科研项目(202102)。

摘　　要：目的建立高效液相色谱-二极管阵列检测器法(HPLC-DAD)测定头孢噻肟钠中基因毒性杂质2-巯基苯并噻唑(MBT)的含量。方法采用Agilent SB-AQ C18柱(250 mm×4.6 mm,5μm),流动相A:0.025 mol/L磷酸二氢钠(pH 4.5),流动相B:乙腈,采用梯度洗脱,流速1.0 ml/min,柱温30℃,检测波长323 nm,自动进样器温度4℃,进样体积100μl。结果MBT在0.0895~3.7275μg/ml范围内呈良好的线性关系(r=1.0000),检测限为2.0 ng/ml,定量限为6.0 ng/ml,平均回收率(n=9)为98.7%。结论该方法专属性好、灵敏度高、准确度高、样品制备简单且检测成本低,可替代质谱法用于测定头孢噻肟钠中MBT含量。Objective To establish a HPLC-DAD method for the determination of genotoxic impurity 2-mercaptobenzothiazole(MBT)in cefotaxime sodium.Methods MBT was separated on a Agilent SB-AQ Cis(250 mm×4.6 mm,5μm)column with mobile phase consisted of 0.025 mol/L sodium dihydrogen phosphate(pH 4.5)and acetonitrile by gradient elution at the flow rate of 1.0 ml/min.The detection wavelength was 323 nm,column temperature was 30 C,autosampler temperature was 4℃and injection volume was 100μl.Results The MBT had a good linear relationship in the range of 0.0895 to 3.7275μg/ml(r=1.0000),In addition,the limit of detection for MBT was 2.0 ng/ml,the limit of quantitation was 6.0 ng/ml,and the average recovery rate(n=9)was 98.7%.Conclusion The method has good performance in specificity,sensitivity,accuracy,lower cost,and its sample preparation is very simple,which can be used for determination of MBT in cefotaxime sodium instead of mass spectrometer.

关 键 词：头孢噻肟钠 2-巯基苯并噻唑 基因毒性杂质 高效液相色谱-二极管阵列检测器法 

分 类 号：R978.1[医药卫生—药品] R991[医药卫生—药学]