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

作　　者：范志雄 关东 谢斌 符联昌 姜春来 FAN Zhixiong;GUAN Dong;XIE Bin;FU Lianchang;JIANG Chunlai(Zhuhai Rundu Pharmaceutical Co.,Ltd.,Zhuhai,Guangdong 519041,China)

机构地区：[1]珠海润都制药股份有限公司,广东珠海519041

出　　处：《今日药学》2022年第4期273-277,共5页Pharmacy Today

基　　金：国家新药创制重大专项(2014ZX09101009)。

摘　　要：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.

关 键 词：盐酸去甲乌药碱晶型A制备 晶体表征 X粉末衍射特征衍射峰 红外特征图谱 热重分析 差示扫描量热法 

分 类 号：R97[医药卫生—药品]