【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。更多还原

【Abstract】 Objective: To develop a method for the quantitative determination of ambrisentan. Methods:1H NMR spectra were obtained with a Bruker Ascend TM 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 at δ 6. 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 that1 H NMR can be used in the quantitative determination of ambrisentan without reference substance. The method is reliable,rapid,accurate and simple.更多还原