¹H定量核磁共振波谱法测定二对甲苯磺酸缘生替尼对照品的含量

目的：建立采用¹H定量核磁共振波谱法测定二对甲苯磺酸缘生替尼对照品的含量。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，脉冲宽度为10.0μs，延迟时间为1 s和扫描次数32的条件下采集试样氢谱。结果：以化学位移δ分别为5.31和6.28的二对甲苯磺酸缘生替尼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=0.128 1X-0.000 4，相关系数为0.999 9，含量测定的重复性试验的RSD为0.20%（n=6）。测得二对甲苯磺酸缘生替尼的含量为98.54%。结论：分析结果表明，在没有对照品的情况下，核磁共振波谱法可用于二对甲苯磺酸缘生替尼的含量测定，该方法可行，具有快速、准确、简便的优点。

Objective: To develop ¹H quatitative nuclear magnetic resonance (¹H qNMR) method for the determination of yunsintinib ditosylate. Methods: ¹H qNMR spectroscopy was used in DMSO, with a Bruker Ascend^TM 400 MHz. For each sample,32 scans were recorded with pulses width of 10.0 μs and delay time of 1 s. Results: The integration of proton signals at δ=5.31 for yunsintinib ditosylate and at δ=6.28 for maleic acid was used for the quantification. Linear regression of quantitative peak areas ratio (A_x/A_s, Y) of yunsintinib ditosylatemaleic acid versus mass ratio (W_x/W_s, X) yielded a correlation coefficient of 0.999 9 and regression equation of Y=0.128 1X-0.000 4, the precision RSD was 0.20% (n=6). The contents of yunsintinib ditosylate was 98.54%. Conclusion: The results showed that ¹H qNMR can be used for the quantitative determination of yunsintinib ditosylate without reference substance. This method is reliable,rapid,accurate and simple.

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