核磁共振波谱法测定藁本内酯对照品的含量___

目的：测定藁本内酯对照品的含量。方法：采用核磁共振波谱法。使用Bruker AV-600超导核磁共振谱仪，以氘代氯仿为溶剂、测定温度300 K、脉冲宽度13.8 μs、延迟时间2 s和扫描次数8的条件下采集试样氢谱。结果：以化学位移分别在δ6.25、δ6.40处的藁本内酯和香豆素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 = 0.0263+0.6676x，相关系数为r = 0.9991，含量测定重复性试验的RSD为0.44%(n = 6)。测得3批藁本内酯对照品的绝对含量分别为87.34%，88.63%，90.25%。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藁本内酯的含量测定，该方法可行，具有快速、准确、简便的优点。

Objective: To develop a method for the quantitative determination of ligustilide. Method: 1H NMR spectra were obtained in CDCl3 with a Bruker AV-600 MHz spectromrter at 300K. For each sample, 8 scans were recorded with pulses width 13.8 μs and delay time 2 s. Results: The integration of proton signals atδ6.25 of ligustilide and δ6.40 of coumarin could be used for the quantification. Linear regression of quantitative peak areas ratio (As/As, y) of ligustilide-coumarin versus mass ratio (ms/mr, x) yielded a correlation coefficient of 0.9991 and regression equation of y = 0.0263+0.6676x, the precision RSD is 0.44% (n = 6). The contents of 3 batchs ligustilide were 87.34%，88.63%，90.25%，respectively．Conclusion: The results showed that 1H NMR can be used for the quantitative determination of ligustilide without reference substance. This method was reliable, rapid, accurate and simple.