摘要
目的:研制聚乙二醇标准物质,为标示聚乙二醇分子量及分布、加强质量控制提供依据。方法:采用IR,NMR,MS等技术对聚乙二醇4000结构进行确认,费休氏法测定水分,TGA法考察炽灼残渣,DVS法考察引湿性,建立了HPLC-CAD法快速对比批间原料的差异,用于筛选原料。分别采用单因素方差分析及直线拟合法对分子量进行了均匀性及稳定性考察,采用多家实验室协作标定的方法对特性量值重均分子量进行定值。结果:研制的聚乙二醇4000具有良好的均匀性和稳定性,重均分子量为3798。结论:首次研制了聚乙二醇4000分子量及分布研究用标准物质,明确了此类标准物质研制思路,并完成了多次换批工作。
Objective:To develop the national pharmaceutical reference standards of polyethylene glycol 4000 for marking the molecular weight and distribution,improving the standard of quality control.Methods:The structure of polyethylene glycol 4000 was confirmed by IR,NMR,MS and other techniques.The moisture content was determined by Karl-Fischer titration method.The ignition residue was investigated by TGA method,and the hygroscopicity was investigated by DVS method.To screen the raw materials,the HPLC-CAD method was established to quickly compare the differences between batches of raw materials.The uniformity and stability of molecular weight were investigated by single-factor analysis of variance and linear fitting method,respectively.The weightaverage molecular weight of the characteristic value was determined by the method of collaborative calibration of multiple laboratories.Results:The polyethylene glycol 4000 has good uniformity and stability,and the Mw is 3798.Conclusion:The reference material for the study of molecular weight and distribution of polyethylene glycol 4000 was developed for the first time.The development strategy of this kind of reference material was clarified and a number of batch work were completed.
作者
李樾
孙会敏
杨锐
杨会英
LI Yue;SUN Hui-min;YANG Rui;YANG Hui-ying(NMPA Key Laboratory for Quality Research and Evaluation of Pharmaceutical Excipients,National Institutes for Food and Drug Control,Beijing 100050,China)
出处
《中国新药杂志》
CAS
CSCD
北大核心
2024年第18期1952-1959,共8页
Chinese Journal of New Drugs
关键词
聚乙二醇4000
分子量
分子量分布
凝胶渗透色谱
HPLC-CAD
国家药品标准物质
polyethylene glycol 4000
molecular weight
molecular weight distribution
gel permeation chromatography
HPLC-CAD
national pharmaceutical reference standards
