摘要
目的:建立定性和定量用阿戈美拉汀的首批国家对照品。方法:应用IR光谱、气质联用及NMR技术对阿戈美拉汀进行结构确证。采用HPLC法测定纯度并且对均匀性、稳定性进行研究,并测定干燥失重、炽灼残渣、热重分析等,通过质量平衡法计算阿戈美拉汀含量。结果:确证阿戈美拉汀的结构,确定首批阿戈美拉汀对照品含量为99.9%,与核磁定量法测定的结果、高氯酸非水滴定结果、差示扫描量热法(differential scanning calorimetry, DSC)结果基本一致。结论:首批阿戈美拉汀国家对照品的研制可作为阿戈美拉汀原料及其相关制剂的鉴别和含量测定用对照品。
Objective:To establish the first batch of national reference standard of agomelatine for qualitative and quantitative determination.Methods:The structure of agomelatine was confirmed by IR,NMR an d GC-MS spectroscopy.The purity of agomelatine was determined by HPLC,and the homogeneity and stability were studied.Moreover,the drying weight loss and residual ignition were determined.The content of agomelatine was calculated by mass balance method.Results:The structure of agomelatine was confirmed.The content of agomelatine was assigned as 99.9%,which was basically consistent with the results of nuclear magnetic resonance quantitative method,perchloric acid non-aqueous titration and DSC.Conclusion:The first batch of national reference standard of agomelatine can be applied for the identification and content determination of agomelatine and its related preparations.
作者
孙长迎
文强
张燕霞
尹利辉
SUN Chang-ying;WEN Qiang;ZHANG Yan-xia;YIN Li-hui(China Institutes for Food and Drug Control,Beijing 102629,China;NMPA Key Laboratory for Quality Research and Evaluation of Chemical Drugs,Beijing 102629,China;Jiangsu Hansoh Pharmaceutical Co.,Ltd.,Lianyungang 222000,China)
出处
《中国新药杂志》
CAS
CSCD
北大核心
2024年第14期1482-1488,共7页
Chinese Journal of New Drugs
基金
国家药品监督管理局化学药品质量研究与评价重点实验室科研资助项目:热分析技术在药品对照品研制中的应用研究(2023HYZX26)。
