核磁共振氟谱对五氟利多的定量分析

The quantitative analysis of Penfluridol by 19FNMR

目的建立核磁共振氟谱测定五氟利多定量分析的方法.方法 Varian-300核磁共振谱仪,四核宽带探头,氟谱检测观察频率:282.234 MHz;谱宽:150^-150ppm;脉冲宽度:谱仪的90度脉冲值15μs;增益值:30;采样时间:1s;采样次数:一般32次,浓度低时数百次直到信号峰清晰;样品溶剂为氯仿,毛细管内标含稀释的三氟乙酸。结果氟谱信号峰的积分显示五氟利多在水与盐酸中完全不溶,在氯仿中的溶解度最好。在氯仿中,Varian-300氟谱的灵敏度可以检测出16ppm的五氟利多溶液,但需要合适的检测参数与扫描3 000次。检测不同浓度的氟谱,以毛细管内标标定,获得CF3氟信号峰的相对积分值,作图获得标准曲线,线性关系良好,r=99.95%。标准曲线法测定药片中五氟利多的含量为20.05mg,与说明书的实值20mg基本一致,实验RSD值为0.48%,平均回收率为99.70%。结论测定方法简便快速,结果准确,可以用于未知样品或药片中五氟利多的定量分析.

Objective Study on the quantitative analysis of Penfluridol by 19 F NMR.Methods Varian-300 NMR instrument,with broadband auto-switchable probe,19 Fdetection frequency：282.234 MHz;spectral width：150 –-150ppm;pulse width：15μs,the 90 degree pulse of the instrument;gain value：30;acquisition time：1s;scan time：regularly 32,may increase to hundreds until the F signals becomes clear and intense;solvent：chloroform;reference standard：long capillary tube containing dilute CF3CO2 H.Results The integration of F signals showed that Penfluridol was insoluble in H2 O or HCl,and soluble best in chloroform.The sensitivity test showed that Varian-300 could detect 16 ppm of penfluridol in chloroform at around 3000 scans with optimum parameters.Standard curve was obtained by plotting concentration versus CF3 integration,straight line was observed with excellent fitting,r=99.95%.Penfluridol in pill was determined to be 20.05 mg from standard curve and which was consistent with the true value of 20 mg.Experiments showed that RSD was 0.48% and average recovery was 99.70%.Conclusion This method is accurate and reliable,and can be used to determine the amount of Penfluridol in unknown samples or pills.