反相高效液相色谱法同时测定玛巴洛沙韦原料药中3种立体异构体含量  

Determination of Three Stereoisomers in Baloxavir Marboxil by Reversed-phase HPLC

作　　者：史凯 闫凯 孙婷 冯雪 周付刚 赫玉霞 刘雪莉 朱嘉亮[4] SHI Kai;YAN Kai;SUN Ting;FENG Xue;ZHOU Fugang;HE Yuxia;LIU Xueli;ZHU Jialiang(Zhongqi Pharmaceutical Technology(SJZ)CO.,LTD.,Shijiazhuang 050035,China;Hebei Institute for Drug and Medical Device Control,Shijiazhuang 050200,China;Institute of Medical Engineering and Translational Medicine,Tianjin University,Tianjin 300072,China;National Institutes for Food and Drug Control,Beijing 102629,China)

机构地区：[1]石药集团中奇制药技术(石家庄)有限公司,石家庄050035 [2]河北省药品医疗器械检验研究院,石家庄050200 [3]天津大学医学工程与转化医学研究院,天津300072 [4]中国食品药品检定研究院,北京102629

出　　处：《医药导报》2025年第4期633-638,共6页Herald of Medicine

基　　金：河北省自然科学基金资助项目(H2021329002)。

摘　　要：目的建立同时测定玛巴洛沙韦原料药中3种立体异构体含量的反相高效液相色谱法,为完善该品种的质量标准提供参考。方法采用CHIRALPAK IC-3(4.6 mm×150 mm,3μm)色谱柱;流动相为乙腈-0.1%甲酸溶液-异丙醇(体积比35∶50∶15);柱温40℃;流速0.5 mL·min^(-1);进样量10μL;检测波长259 nm。结果主峰与各立体异构体峰均可达到完全分离;立体异构体1、立体异构体2、立体异构体3的检测限分别为0.0247、0.0387、0.0381μg·mL^(-1),立体异构体1、立体异构体2、立体异构体3的定量限分别为0.0494、0.0773、0.0761μg·mL^(-1);3个杂质在对应的浓度范围内与各自峰面积呈良好线性关系,立体异构体1、立体异构体2和立体异构体3的线性浓度范围分别为0.0495~0.9890μg·mL^(-1),0.0516~1.0310μg·mL^(-1),0.0508~1.0150μg·mL^(-1),线性相关系数均为0.9994;回收率92.28%~103.90%;供试品溶液在室温放置48 h稳定。结论该方法准确、可靠,能够有效地检测玛巴洛沙韦原料药中立体异构体含量,为玛巴洛沙韦原料药质量标准的建立和安全性评价提供参考。Objective To establish a reversed-phase HPLC method for determining three stereoisomers in baloxavir marboxil and provide a basis for the quality specification of baloxavir marboxil.Methods The chromatographic column was CHIRALPAK IC-3(4.6 mm×150 mm,3μm),The mobile phase was acetonitrile-0.1%formic acid aqueous solution-isopropanol(35∶50∶15).The column temperature was 40℃.The flow rate was 0.5 mL·min^(-1).The injection volume was 10μL.The detection wavelength was 259 nm.Result The isomer peaks were completely separated from the principal component peak.The detection limits for stereoisomers 1,2 and 3 were 0.0247,0.0387,0.0381μg·mL^(-1) respectively.The quantitation limits for stereoisomers 1,2 and 3 were 0.0494,0.0773,0.0761μg·mL^(-1) respectively.There were good linear relationships between the concentrations and peak area within the ranges of the study,and the linearity concentration ranges of stereoisomers 1,2 and 3 were 0.0495-0.9890μg·mL^(-1),0.0516-1.0310μg·mL^(-1),0.0508-1.0150μg·mL^(-1) respectively.The linear correlation coefficients were 0.9994.The recovery was 92.28%-103.90%.The sample solution was stable in 48 h at room temperature.Conclusion The method is accurate and reliable for determining stereoisomers in baloxavir marboxil,and provide a guideline of quality standards of baloxavir marboxil and safety evalution.

关 键 词：玛巴洛沙韦 立体异构体 含量测定 反相高效液相色谱法 

分 类 号：R95[医药卫生—药学]