盐酸去甲乌药碱晶型A制备与固态表征

Preparation and Solid-state Characterization of Higenamine Hydrochloride Polymorph A

目的 研究溶液pH值、溶解温度及结晶方式等条件对盐酸去甲乌药碱结晶的影响,并采用阶段控温析晶方法,制备得到盐酸去甲乌药碱晶型A晶体。方法 采用X射线粉末衍射、热重分析、差示扫描量热法和红外光谱等对盐酸去甲乌药碱晶型A晶体进行结构和热力学表征。结果 晶型A化合物具有纯度高、稳定性好、用药安全性高、制剂适用性好等优点,有利于延长盐酸去甲乌药碱药品的有效期。结论 采用阶段控温析晶方法进行结晶处理制备得到盐酸去甲乌药碱晶型A化合物,确保析出的固体为高纯度的目标产物,且在产物中不存在油状物杂质。

OBJECTIVE To investigate the effects of solution pH value,dissolution temperature,and means on crystallization of higenamine hydrochloride,and to obtain higenamine hydrochloride polymorph A using stage-temperature controlled crystallization method.METHODS X-ray power diffraction analysis(XRD),thermogravimertric analysis(TGA),differential scanning calorimetry(DSC),and Fourier transform infrared spectroscopy(FT-IR)were used to characterize solid-state structure and thermodynamic characterizations of higenamine hydrochloride polymorph A.RESULTS The polymorph A compound has the advantages of high purity,good stability,high safety and good preparation applicability,which is beneficial to prolong the term of validity of the drug.CONCLUSION Stage-temperature controlled crystallization method was used to prepare high-pure higenamine hydrochloride polymorph A products,and no any oil-like impurities were in the products.