摘要
采用核磁共振波谱法对利托那韦片进行定性鉴别和定量分析。核磁共振氢谱(^(1)HNMR)、核磁共振碳谱(13CNMR)、无畸变极化转移增强(DEPT-135)、异核单量子相干谱(HSQC)等对利托那韦片成分进行鉴别。选择利托那韦化学位移8:8.91~8.99ppm处为定量峰,对苯二甲酸二甲酯化学位移8:8.07~8.18ppm处为内标峰,采用定量核磁共振氢谱(qHNMR)测定利托那韦片含量。HNMR、13CNMR、DEPT-135和HSQC结果显示,利托那韦片中成分的化学结构与利托那韦结构式相符。qHNMR方法学专属性高,利托那韦线性范围为5.69~20.02mg·mL^(-1),精密度及稳定性良好,平均回收率为100.77%,qHNMR法测得利托那韦片含量与HPLC法测得结果基本一致。所以建立分析方法可用于利托那韦片定性鉴别和定量分析,为利托那韦片提供了一种准确、快速、简便的质量控制方法。
Nuclear magnetic resonance spectroscopy was employed for qualitative identification and quantitative analysis of ritonavir tablet.Component of ritonavir tablet was identified by hydrogen nuclear magnetic resonance(^(1)HNMR),carbon nuclear magnetic resonance(13CNMR),distortionless enhancement by polarization transfer(DEPT-135)and heteronuclear single quantum coherence(HSQC).Proton signal peaks at 8:8.91~8.99 ppm of ritonavir and 3:8.07~8.18 ppm of dimethyl terephthalate were employed as quantitative peak and internal standard peak,quantitative hydrogen nuclear magnetic resonance(qHNMR)was used to determine content of ritonavir tablet.Results of'HNMR,13CNMR,DEPT-135 and HSQC showed that the chemical structure of component was consistent with that of ritonavir.Specificity of qHNMR was high,linear range of ritonavir was 5.69~20.02 mg mL^(-1),precision and stability were good,and average recovery was 100.77%.The content of ritonavir tablet determined by qHNMR was generally consistent with those of HPLC method.Therefore,the established analytical methods could be used for qualitative identification and quantitative analysis of ritonavir tablet,which provided an accurate,rapid and simple method for the quality control of ritonavir tablet.
作者
王江洪
宋亚男
李莹
王玉洁
决利利
郑严
赵新永
WANG Jiang-hong;SONG Ya-nan;LI Ying;WANG Yu-jie;JUE Li-Li;ZHENG Yan;ZHAO Xin-yong(Department of Medical Laboratory,Medical College,Zhengzhou University of Industrial Technology,Zhengzhou 451100,China;Shanghai Zhangjiang Yaogu Public Service Platform Co.,Ltd.,Shanghai 201203,China)
出处
《化学研究与应用》
CAS
北大核心
2024年第6期1349-1355,共7页
Chemical Research and Application
基金
2023年度河南省高等学校重点科研项目计划(23B310010)资助。
关键词
利托那韦片
定量核磁共振氢谱
定性鉴别
定量分析
ritonavir tablet
quantitative hydrogen nuclear magnetic resonance
qualitative identification
quantitative analysis
作者简介
通讯联系人:赵新永(1969-),男,博士,副教授,主要从事药物研发。E-mail:309525071@qq.com。
