聚乙二醇4000国家药品标准物质的研制
Establishment of the national pharmaceutical reference standards of polyethylene glycol 4000
李樾 1孙会敏 1杨锐 1杨会英1
作者信息
- 1. 国家药品监督管理局药用辅料质量研究与评价重点实验室,中国食品药品检定研究院,北京 100050
- 折叠
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3 798.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.
Abstract
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 weight-average 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 3 798.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.
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Key words
polyethylene glycol 4000/molecular weight/molecular weight distribution/gel permeation chromatography/HPLC-CAD/national pharmaceutical reference standards引用本文复制引用
出版年
2024
NETL
NSTL
万方数据