高效液相色谱法同时测定甲苯磺酸妥舒沙星中4种遗传毒性杂质的含量  

Simultaneous determination of 4 genotoxic impurities in tosufloxacin tosylate hydrate by HPLC

作　　者：陈鸿玉 程雪清 廖漾 周碧红 刘栋华 刘雁鸣 李昌亮 CHEN Hong-yu;CHENG Xue-qing;LIAO Yang;ZHOU Bi-hong;LIU Dong-hua;LIU Yan-ming;LI Chang-liang(Hunan Institute for Drug Control,Hunan Engineering&Technology Research Center for Pharmaceutical Quality Evaluation,Key Laboratory of Pharmaceutical Excipients Engineering Technology of State Drug Administration,Changsha 410001;Hinye Pharmaceutical Co.,Ltd.,Hunan Osteoarthritis Drug Engineering Technology Research Center,Hunan Engineering&Technology Research Center for Pharmaceutical Quality Evaluation,Changsha 410331;Hinye Pharmaceutical Co.,Ltd.,Changsha 410331)

机构地区：[1]湖南省药品检验检测研究院,湖南省药品质量评价工程技术研究中心,国家药品监督管理局药用辅料工程技术研究重点实验室,长沙410001 [2]天地恒一制药股份有限公司,湖南省骨关节疾病药物工程技术研究中心,湖南省药品质量评价工程技术研究中心,长沙410331 [3]天地恒一制药股份有限公司,长沙410331

出　　处：《中南药学》2022年第12期2901-2905,共5页Central South Pharmacy

基　　金：湖南科药联合基金项目(No.2021JJ80003)。

摘　　要：目的采用高效液相色谱(HPLC)法同时测定甲苯磺酸妥舒沙星中4种遗传毒性杂质(2,4-二氟苯胺、2,6-二氟苯胺、对甲苯磺酸甲酯和对甲苯磺酸乙酯)的含量。方法采用CAPCELL PAK C18柱(4.6 mm×250 mm,5μm)色谱柱;流动相为乙腈-水,梯度洗脱;柱温为35℃;流速为0.8 mL·min^(-1);检测波长为225 nm。结果2,4-二氟苯胺、2,6-二氟苯胺、对甲苯磺酸甲酯和对甲苯磺酸乙酯质量浓度分别在0.0404~0.6064μg·mL^(-1)(r=0.9997)、0.0282~0.6055μg·mL^(-1)(r=0.9998)、0.0403~0.6045μg·mL^(-1)(r=0.9997)、0.0401~0.6019μg·mL^(-1)(r=0.9999)与峰面积呈良好的线性关系,平均加样回收率在95.9%~101.3%,RSD在0.40%~7.3%。结论该方法专属性强,重复性好,准确度高,可为甲苯磺酸妥舒沙星的质量控制及标准研究提供参考。Objective To simultaneously determine 4 genotoxic impurities(2,4-difluoroaniline,2,6-difluoroaniline,methyl p-toluenesulfonate and ethyl p-toluenesulfonate)in tosufloxacin tosylate hydrate by HPLC.Methods The determination was performed on a CAPCELL PAK C18(4.6 mm×250 mm,5μm)column,and the mobile phase was acetonitrile-water with gradient elution at 0.8 mL·min^(-1).The column temperature was 35℃.The detection wavelength was 225 nm.Results The concentration of 2,4-difluoroaniline,2,6-difluoroaniline,methyl p-toluenesulfonate and ethyl p-toluenesulfonate was 0.0404~0.6064μg·mL^(-1)(r=0.9997),0.0282~0.6055μg·mL^(-1)(r=0.9998),0.0403~0.6045μg·mL^(-1)(r=0.9997),and 0.0401~0.6019μg·mL^(-1)(r=0.9999),with a good linearity in the peak area.The average recovery was at 95.9%~101.3%with RSD at 0.40%~7.3%,respectively.Conclusion The method is validated,with strong specificity,good repeatability and high accuracy,which can provide reference for the quality control and standard research of tosufloxacin tosylate hydrate.

关 键 词：高效液相色谱法 甲苯磺酸妥舒沙星 遗传毒性杂质 

分 类 号：R927[医药卫生—药学]