摘要
目的:尝试制备满足单晶X射线衍射法(single crystal X-ray diffraction,SCXRD)测定要求的头孢他啶单晶体并测定其晶体结构。方法:采用冷却法在水溶液中制备头孢他啶晶体,利用SCXRD测定其晶体结构,并采用差示扫描量热法和拉曼光谱法对其进行表征。结果:制备了大小合适,质量好的头孢他啶晶体。晶体结构测定结果显示,晶胞中含有4个头孢他啶分子和20个水分子,其化学计量式为C22H32N6O12 S2·5H2O,晶态下分子内不存在氢键联系,分子间存在氢键联系。结论:该单晶体制备方法成熟可靠、重现性好,制备得到的头孢他啶晶体可用于结构测定,测得晶体结构以及表征图谱为头孢他啶晶型相关研究提供了基础数据和技术参考。
Objective:To prepare ceftazidime crystal which satisfies the requirement for precise determination of the crystal form by single crystal X ray diffraction(SCXRD).Methods:Ceftazidime crystal was prepared in water solution by cooling method.Crystal structure was obtained by SCXRD.And the crystal prepared was characterized by differential scanning calorimetry and Raman spectroscopy.Results:The crystal prepared was suitable for SCXRD determination.It was shown that there were four ceftazidime molecular and twenty H2O molecular in a single crystal lattice.The stoichiometric formula is C22 H32 N6O12 S2·5H2O.There are no intramolecular hydrogen bonds while there are intermolecular hydrogen bonds.Conclusion:The developed method for preparing ceftazidime crystal is sophisticated,reliable and reproducible,which is suitable for SCXRD determination.Both DSC pattern and Raman spectra of the ceftazidime crystal provide useful information and technical references for further research of polymorph of this drug.
作者
王琰
张斗胜
田冶
孟红梅
张彦民
刘飞
胡昌勤
邹文博
许明哲
WANG Yan;ZHANG Dou-sheng;TIAN Ye;MENG Hong-mei;ZHANG Yan-min;LIU Fei;HU Chang-qin;ZOU Wen-bo;XU Ming-zhe(National Institutes for Food and Drug Control,Beijing 102629,China;Department of Neurology and Neuroscience Center,First Hospital of Jilin University,Changchun 130021,China;School of Pharmacy,Health Science Center,Xi'an Jiaotong University,Xi'an 710061,China;Shandong Center for Food and Drug Evaluation&Certification,Jinan 250014,China)
出处
《中国新药杂志》
CAS
CSCD
北大核心
2020年第15期1764-1769,共6页
Chinese Journal of New Drugs
基金
国家“重大新药创制”科技重大专项资助项目(2017ZX09101001-007)。
关键词
头孢他啶
晶体制备
晶体结构测定
ceftazidime
crystal preparation
crystal structure determination
