核磁共振氟谱法测定氟他胺含量的实验设计

Experimental Design for Determination of Flutamide by 19F NMR Spectroscopy

设计了核磁共振氟谱法(19F NMR)测定氟他胺含量的实验。此实验以三氟甲苯为内标,化学位移δ=-61.10×10^-6 处的氟他胺的特征峰作为定量峰。实验结果表明,氟他胺的19F NMR检测方法在其浓度0.2~10.0 mg/mL范围内,样品与内标物的积分面积比与浓度比具有良好的线性关系(R^2=0.996)。实验方法的定量限和检出限分别为18 μg/mL和5 μg/mL;同一标准品溶液重复实验5次,相对标准偏差(RSD)为1.94%,证明该方法重复性比较好。此实验不仅为氟他胺的定量分析提供了一种实用、快速有效的方法,而且培养了学生的创新思维和科研能力。

A method for the determination of flutamide by 19F NMR spectroscopy was established in this work. Benzo-trifluoride was employed as the internal standard,and the characteristic peak with δ of -61.10×10^-6 ,assigned to flutamide was selected as the quantitative peak. The experimental results showed that there is a good linear relationship (R^2 = 0.996) between the integral ratio of flutamide to benzo-trifluoride and their concentration ratio when the concentration of flutamide was within the range of 0.2-10.0 mg/mL. The limits of quantitaion (LOQ) and limit of determination (LOD) of 18 and 5 μg/mL were obtained,respectively. The relative standard deviation (RSD) of five replicates is 1.94%,revealing the excellent repeatability of the proposed method. It is proved that this experiment not only provides a practical,rapid and efficient way for quantitative analysis of flutamide,but also effectively cultivates students’ creative thinking and scientific research ability.