摘要
采用核磁共振氟谱检测盐酸氟西汀,在δ14.15出现信号峰,随着浓度减小(2.00～0.05 mmol.L1),化学位移略往高场移动(δ14.158到14.145),定性分析的进一步确定可以采用盯梢重叠实验。氟谱灵敏度可以达到17 mg.L1,符合药典要求,但需要扫描500次与使用合适的参数。定量分析上制作出浓度氟谱积分的标准工作曲线,藉由内插或公式法进行快速定量分析。氟标准曲线的制作中,本文提出使用毛细管内标法,利用毛细管中的三氟乙酸作为积分的标定参考。此法操作简便并获得极佳的线性拟合度;使用三氟乙醇直接添加法制作的标准曲线的线性拟合度不如预期。
The chemical shift of fluoxetine hydrochloride appears at δ 14.15 in 19F NMR analysis.The δ moved upfield slightly from 14.158 to 14.145 when the concentration of solution became diluted from 2.00 to 0.05 mmol-L-1.Spiking test was suggested to confirm the existence of the compound for qualitative analysis.19F NMR detection sensitivity test illustrated that a concentration of 17 mg in 1 L water could be detected while the sample was scanned 500 times with optimum parameters.In quantitative analysis,standard curve of concentration versus fluorine signal intensity was proposed to determine the amount of fluoxetine.Long capillary tube containing trifluoroacetic acid was used as internal standard for the integration measurements and straight line was obtained with good fitting.Direct additions of trifluoroethanol to fluoxetine solutions gave a poorer standard curve.
出处
《药学学报》
CAS
CSCD
北大核心
2012年第5期630-633,共4页
Acta Pharmaceutica Sinica
关键词
盐酸氟西汀
核磁共振氟谱
三氟乙酸
fluoxetine hydrochloride
19F NMR
trifluoroacetic acid
