杨百勤 孔二丽 薛潇迪 赵寿骞 林崇熙. 采用核磁共振氟谱定性与定量分析盐酸氟西汀J. 药学学报, 2012,47(5): 630-633.
引用本文: 杨百勤 孔二丽 薛潇迪 赵寿骞 林崇熙. 采用核磁共振氟谱定性与定量分析盐酸氟西汀J. 药学学报, 2012,47(5): 630-633.
YANG Bai-Qin, Kong-Er-Li, Xue-Xiao-Di, Zhao-Shou-Jian, Lin-Chong-Xi. Qualitative and quantitative analysis of fluoxetine hydrochloride by 19F NMRJ. 药学学报, 2012,47(5): 630-633.
Citation: YANG Bai-Qin, Kong-Er-Li, Xue-Xiao-Di, Zhao-Shou-Jian, Lin-Chong-Xi. Qualitative and quantitative analysis of fluoxetine hydrochloride by 19F NMRJ. 药学学报, 2012,47(5): 630-633.

采用核磁共振氟谱定性与定量分析盐酸氟西汀

Qualitative and quantitative analysis of fluoxetine hydrochloride by 19F NMR

  • 摘要:

    采用核磁共振氟谱检测盐酸氟西汀, δ 14.15出现信号峰, 随着浓度减小 (2.000.05 mmol·L−1), 化学位移略往高场移动 (δ 14.15814.145), 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·L−1, 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。

     

    Abstract:

    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.

     

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