盐酸地芬尼多中1,3-二哌啶丙烷的合成及气相色谱方法建立

Synthesis and Determination of 1,3-dipiperidine Propane in Difenidol Hydrochloride by Gas Chromatography Spectrometry

目的建立盐酸地芬尼多片中杂质1,3-二哌啶丙烷的检测方法。方法采用Agilent DB-624气相柱(30 m×0.25 mm,1.0μm),程序升温,以甲醇为溶剂,检测器为氢火焰离子化检测器。结果1,3-二哌啶丙烷在0.1 mg·mL^(-1)~2 mg·mL^(-1)浓度范围内呈良好的线性关系,最低检测限、定量限分别为0.001 mg·mL^(-1)、0.005 mg·mL^(-1),加样回收率在98.1%~101.8%之间。结论经方法学验证,本法专属性强、灵敏度高、准确度高,可用于盐酸地芬尼多中1,3-二哌啶丙烷测定,为其质量控制提供方法保证。

OBJECTIVE A method for the detection of 1,3-dipyridine propane in diffenidol hydrochloride was established.METHODS Agilent DB-624 capillary column(30 m×0.25 mm,1.0μm)was used,temperature programmed,methanol as solvent and hydrogen flame ionization detector as detector.RESULTS 1,3-dipyridine propane showed a good linear relationship in the range of 0.1 mg·mL^(-1)~2·mL^(-1).The minimum detection limit and quantitative limit were 0.001 mg·mL^(-1) and 0.005 mg·mL^(-1) respectively.The recovery was 98.1%~101.8%.CONCLUSION The method has strong specificity,high sensitivity and high accuracy.It can be used for the determination of 1,3-dipyridine propane in difenidol hydrochloride and provide a method guarantee for its quality control.