高效凝胶渗透色谱法测定聚乙二醇分子量及其分布  

Determination of Molecular Weight and Its Distribution of Polyethylene Glycol by High Performance Gel Chromatography

作　　者：程继业 周震宇 金伟斌 陈礼峰 姚玲 CHENG Ji-ye;ZHOU Zhen-yu;JIN Wei-bin;CHEN Li-feng;YAO Ling(Suzhou Institute for Drug Control,Suzhou 215104,China)

机构地区：[1]苏州市药品检验检测研究中心,苏州215104

出　　处：《中国合理用药探索》2022年第10期97-103,共7页Chinese Journal of Rational Drug Use

基　　金：国家药典委员会药品标准制修订研究课题(ZG2018-5-5)。

摘　　要：目的:建立聚乙二醇(PEG)分子量及分布的测定方法,比较3家企业共9批样品的质量差异,为药用辅料质量标准提高提供依据。方法:采用Agilent PL aquagel-OH 20凝胶渗透色谱柱、示差折光检测器进行分离分析,流动相为0.1mol/L硝酸钠溶液(含0.02%ProClin^(TM));流速为0.5ml/min;柱温为35℃;检测器温度为35℃;进样体积为100μl。建立三阶校正曲线,通过Empower 3 GPC软件计算各样品的分子量及分布结果。结果:PEG分子量在430~5800范围内时线性关系良好,各校正点平均偏差均在98%~102%之间,可准确测定9批PEG样品的数均分子量(Mn)、重均分子量(Mw)以及分布系数等分子量分布信息。结论:高效凝胶渗透色谱(GPC)方法是测定PEG分子量及分布的可靠方法,用于评价高分子化合物多分散属性时具有结果准确、重现性高等优点,结合累计分布曲线相关信息可用于多批样品的质量控制和比对。在一定程度上为药品研发中辅料的筛选以及国家标准的提高提供了依据。Objective:To establish a method for the determination of molecular weight and distribution of polyethylene glycol(PEG),and compare the quality diff erences of nine batches of samples from three enterprises,so as to provide a basis for improving the quality standard of pharmaceutical excipients.Methods:The Agilent PL aquagel-OH gel chromatography column and diff erential refractive index detector were used for separation and analysis.The mobile phase was 0.1 mol/L sodium nitrate solution(containing 0.02%ProClin^(TM))with fl ow rate of 0.5ml/min,column temperature of 35°C,detector temperature of 35°C and injection volume of 100μl.The three order calibration curve was established and the molecular weight and distribution results of the products were calculated by waters Empower GPC system.Results:The linear relationship is good in the range of molecular weight 430-5800of polyethylene glycoland the average deviation of correction point was within 98%~102%.It can accurately determine the molecular weight distribution information of the average molecular weight(Mn),heavy average molecular weight(Mw)and distribution coefficient of 9 batches of PEG samples.Conclusion:High performance gel permeation chromatography(GPC)is a reliable method for the determination of molecular weight and distribution of polyethylene glycol.It has the advantages of accuracy and high reproducibility when used to evaluate the polydispersity properties of macromolecular compounds.Combined with relevant information of cumulative distribution curves,it can be used for quality control and comparison of multiple batches productsand provide a basis for the selection of excipients in drug development and improvement of national drug standards.

关 键 词：聚乙二醇 分子量 分子量分布 高效凝胶渗透色谱 多分散性 

分 类 号：O657.7[理学—分析化学]