分析测试学报2017,Vol.36Issue(11):1312-1317,6.DOI:10.3969/j.issn.1004-4957.2017.11.004
超高效凝胶色谱法测定聚乙二醇衍生物的分子量及其分布
Determination of the Molecular Weight and Molecular Weight Distribution of Polyethylene Glycol Derivatives by Advanced Polymer Chromatography
摘要
Abstract
A method of advanced polymer chromatography (APC) was established for the determination of the molecular weights and their distributions of polyethylene glycol derivatives and the impurity contents,with monomethoxy polyethylene glycol propyl aldehyde (mPEG_ pALD) as the representation for polyethylene glycol derivatives.The chromatographic conditions such as chromatographic column and mobile phase were optimized,while the effects of the concentration of sample (within the concentration range of 0.5-20 mg/mL) and dissolution time were also investigated.The optimized chromatographic conditions were as follows:three ultra-high performance gel columns were connected in series at 40 ℃ with methanol-water (95 ∶ 5,by volume) as mobile phase at a flow rate of 0.5 mL/min,and a refractive index detector was selected.The result showed that the weight-averaged molecular weight(Mw) of mPEG_ pALD was 19 444 and its distribution index(D) was 1.01,while the Mw for impurity 1 was 38 703 with its D index of 1.01 and its content of 1.31%,and the Mw for impurity 2 was 61 036 with its D index of 1.00 and its content of 0.70%.Compared with the traditional GPC method,this APC method could obtain the molecular weight and its distribution of mPEG_ pALD with higher resolution and less time,and the content of impurity could also be acquired.The method provides a scientific basis for the research,development and quality control of PEG derivatives,and is applicable for the determination of molecular weight,molecular weight distribution and purity of other PEG derivatives.关键词
超高效凝胶色谱法/聚乙二醇衍生物/相对分子量/杂质含量/单甲氧基聚乙二醇丙醛Key words
ultra high performance gel chromatography/polyethylene glycol derivatives/relative molecular weight/impurity content/mPEG_pALD分类
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谢梦婷,黄晓兰,罗辉泰,黄芳,朱志鑫,李兴,吴惠勤..超高效凝胶色谱法测定聚乙二醇衍生物的分子量及其分布[J].分析测试学报,2017,36(11):1312-1317,6.基金项目
广东省科学院科研平台环境与能力建设专项资金项目(2016GDASPT-0308) (2016GDASPT-0308)