机械化学法制备亚稳态7-羟基异黄酮溶剂合物多晶型  

Preparation of Metastable Solvatomorphism of 7-Hydroxyisoflavone by Mechanical Chemical Method

作　　者：刘梅菊 谢逸菲 邹瑶 喻红梅 周健[1] 龚宁波[1] 吕扬[1] LIU Meiju;XIE Yifei;ZOU Yao;YU Hongmei;ZHOU Jian;GONG Ningbo;LYU Yang(Beijing Key Laboratory of Polymorphic Drugs,Institute of Materia Medica,Chinese Academy of Medical Sciences and Peking Union Medical College,Beijing 100050,China;Beijing Key Laboratory of Drug Target Identification and Drug Screening,Institute of Materia Medica,Chinese Academy of Medical Sciences and Peking Union Medical College,Beijing 100050,China)

机构地区：[1]北京协和医学院,中国医学科学院药物研究所,晶型药物研究北京市重点实验室,北京100050 [2]北京协和医学院,中国医学科学院药物研究所,国家药物筛选中心,北京100050

出　　处：《医药导报》2023年第7期959-964,共6页Herald of Medicine

基　　金：北京市自然科学基金资助项目(7222261);中国医学科学院医学与健康科技创新工程资助项目(2022-I2M-1-015,2022-I2M-JB-010);山东省重点研发项目(2021ZDSYS26);国家药典委员会标准提高项目(2022Y01)。

摘　　要：目的系统研究7-羟基异黄酮溶剂合物多晶型现象,为该药开发过程中可能存在的溶剂合物晶型杂质成分的控制提供科学依据。方法通过分析已获得的7-羟基异黄酮溶剂合物结构特点、堆积方式和相互作用,采用机械化学法制备获得2种新的7-羟基异黄酮溶剂合物,采用单晶X射线衍射分析、粉末X射线衍射分析、差示扫描量热分析、热重分析、红外光谱分析对多晶型进行表征,并考察晶型稳定性。结果制备获得的2种7-羟基异黄酮溶剂合物均为亚稳定晶型。结论利用机械化学法可以制备发现亚稳定多晶型,这将为丰富多晶型的种类和晶型的质量控制提供物质基础和技术支撑。Objective To systematically study the solvatomorphism of 7-hydroxyisoflavone and to provide a scientific basis for the quality control of the solvated polymorphic impurities in this drug.Methods By analyzing the structure characteristics,crystal packing,and interactions of the obtained 7-hydroxyisoflavone solvates,two new solvates of 7-hydroxyisoflavone were prepared by mechanical chemical method.Single crystal X-ray diffraction,powder X-ray diffraction,differential scanning calorimeter,thermo gravimetric analysis and infrared spectroscopy were used to characterize the solvates.Furthermore,the stability of solvates was investigated.Results The two new solvates of 7-hydroxyisoflavone prepared in this work were all metastable crystal forms.Conclusion The metastable crystal forms can be prepared by mechanical chemical methods,providing new materials and technical support for enriching the types and the quality control of crystal forms.

关 键 词：7-羟基异黄酮 机械化学法 溶剂合物 多晶型现象 晶体结构 

分 类 号：R917[医药卫生—药物分析学] TQ460.1[医药卫生—药学]