水溶性凝胶渗透色谱法测定聚乙烯亚胺的分子量及其分布讲义.doc

水溶性凝胶渗透色谱法测定聚乙烯亚胺的分子量及其分布 刘瑞鹏*，曾宪海，隋国红，赵金铠 （青岛迪爱生精细化学有限公司 山东 青岛 266101） 摘要：应用水溶性凝胶渗透色谱法测定了聚乙烯亚胺（PEI）的分子量，测试结果与厂家提供结果基本一致。色谱柱0.2~0.3 mol/L 的乙酸-乙酸钠缓冲溶液（pH 4.5~6.0）。系统考察了不同流动相及其pH值，离子强度和进样量对PEI在凝胶柱上吸附等导致的对分析结果的影响。结果发现：增大流动相离子强度有利于减少PEI的吸附，但流动相的pH值对于PEI的吸附具有更重要的影响。该方法具有优良的准确性和重复性。 关键词：水溶性凝胶渗透色谱法，聚乙烯亚胺，分子量及其分布，准确性，重复性 Determination on Molecular Weight and Distribution of Polyethyleneimine with Aqueous Gel Permeation Chromatography LIU Ruipeng, ZENG Xianhai, SUI Guohong, ZHAO Jinkai (Qingdao DIC Fine Chemicals Co. LTD Shandong Qingdao 266101) Abstract：The molecular weight and distribution of polyethyleneimine (PEI) polymers, a series of macromolecular material from Nippon shokubai, was separated by aqueous gel permeation chromatography on PL aquagel-OH 30, PL aquagel-OH 30 and PL aquagel-OH 40 columns and calibrated by universal polyethylene glycol standard. The mobile phase was 0.2-0.3 mol/L acetic acid-sodium acetate buffers with pH value of 4.5-6.0. The measured molecular weight was similar to the actual molecular weight given by the manufacturer. The influence of the sorts of mobile phase and its pH value, ionic strength and the injection volume on the adsorption of the samples by the columns were systematically examined. It was found that the pH value and the ion strength of mobile phase affected the accuracy and reproducibility of the results causing mainly by adsorption of PEI greatly. The increases of pH value and ion strength caused the decrease of adsorption, and moreover, the pH value proved to be a more important factor. The reproducibility of measuring molecular weight and distribution of PEI was controlled within the range of tolerance. Key words：Aqueous Gel Permeation Chromatography, Polyethyleneimine, Molecular Weight and its Distribution, Accuracy, Reproducibility 1 前言 聚乙烯亚胺(PEI)是一种广泛使用的高分子材料，可用作造纸助剂、粘合材料及其助剂、涂料及墨水助剂、纺织助剂和分散剂等。此外，聚乙烯亚胺是1995年发现的重要的非病毒核酸载体1，由于具有价格低、操作简单、安全性高等特点而备受关注，是目前应用最广泛的非病毒载体之一。聚乙烯亚胺的组成如分子量大小和分布对其各种应用性能有重要影响，但其分子量及其分布测定有许多困难。常用的黏度法