核磁共振波谱法测定安立生坦对照品的含量  

Determination of Ambrisentan Reference Substance by 1 H-Nuclear Magnetic Resonance Spectroscopy

作　　者：仲艳[1] 陈保来[1] 李家春[2] 黄文哲[1] 王振中[1] 萧伟[1] 

机构地区：[1]江苏康缘药业股份有限公司,江苏连云港222047 [2]中国药科大学

出　　处：《中国药师》2015年第5期750-752,共3页China Pharmacist

摘　　要：目的:建立测定安立生坦对照品含量的方法。方法:采用核磁共振波谱法,使用Bruker Ascend TM 400超导核磁共振谱仪,以氘代DMSO为溶剂,在脉冲宽度10.0μs,延迟时间5 s和扫描次数16的条件下采集试样氢谱。结果:以化学位移分别为6.16 ppm和6.28 ppm的安立生坦和顺丁烯二酸的氢质子峰作为定量峰,其峰面积比与其质量比的线性回归方程为Y=0.140 7X+0.034 8,相关系数为0.999 4,含量测定重复性试验的RSD为0.2%(n=6)。测得安立生坦对照品的绝对含量为99.9%。结论:分析结果表明,在没有对照品的情况下,该方法可行,且具有快速、准确、简便的优点。Objective：To develop a method for the quantitative determination of ambrisentan. Methods： 1 H NMR spectra were obtalned with a Bruker AscendTM 400 superconducting NMR spectrometer. For each sample, DMSO-D6 was used as the solvent, the pulse width was 10. 0 μs, the delay time was 5 s and the scanning time was 16. Results： The proton peaks of ambrisentan at δ6. 16 ppm and maleic acid atδ6. 28 ppm were used as the quantitative peaks. The linear regression equation of peak area and quality ratio was Y=0. 140 7X＋0. 034 8 with the correlation coefficient of 0. 999 4. RSD was 0. 2%（n=6）in the repeated experiments. The absolute content of ambrisentan reference substance was 99. 9%. Conclusion： The results showed that 1 H NMR can be used in the quantitative determination of ambrisentan without reference substance. The method is reliable, rapid, accurate and simple.

关 键 词：核磁共振 内标法 安立生坦 含量测定 

分 类 号：R927.2[医药卫生—药学]