核磁共振波谱法测定藁本内酯对照品的含量

Quantitative determination of ligustilide by ~1H-nuclear magnetic resonance spectroscopy

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13.8μs、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 300 K.For each sample,8 scans were recorded with pulses width 13.8μs and delay time 2 s.Results：The integration of proton signals atδ6.25 of ligustilide andδ6.40 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 was 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 is reliable,rapid,accurate and simple.