凝胶排阻色谱法测定中空纤维超滤膜组件对聚乙二醇的截留率

Determination of Polyethylene Glycol Retention Rate of Hollow Fiber Ultrafiltration Membrane Module by Size Exclusion Chromatography

采用凝胶排阻色谱法测定中空纤维超滤膜组件对聚乙二醇20000（PEG20000） 溶液的截留率,选择AgilentPL aquagel-OH MIEXD–H8 μm 色谱柱,流动相为0.1 mol/L NaNO3 溶液 （ 含0.02%NaN3）,流量为1 mL/min,RID 检测器,柱温箱和检测器温度均为30℃.当进样体积为50 μL 时,方法的检出限为18.8 mg/L,定量限为49.0 mg/L.PEG20000 溶液的质量浓度在60～1 000 mg/L 范围内与色谱峰高呈良好的线性,相关系数r^2=1.000.该方法对实际样品测定结果的相对标准差为1.31% （n=6）.将该方法的测定结果与紫外– 可见分光光度计法的测量结果进行F 检验和t 检验,结果表明两种方法测量结果无显著性差异.采用该方法可以同时对PEG20000 样品的相对分子质量及其分布进行测定,从而对选用的截留标准物质进行质量控制.

The method for determining polyethylene glycol （PEG）retention rate of hollow fiber ultrafiltrationmembrane module by high performance size exclusion chromatography （SEC） was established. An Agilent PL aquagel-OH MIEXD–H 8 μm column was used,and the chromatographic conditions were as follows： the mobile phase was0.1 mol/L NaNO3 solution （with 0.02% NaN3） with flow rate of 1 mL/min,RID detector was selected and thetemperature of the column and detector was 30℃ . The detection limit of the method was 18.8 mg/L and quantificationlimit was 49.0 mg/L as single injection volume was 50μL. The concentration of PEG20000 was linear with peakheight in the range of 60–1 000 mg/L and the linear correlation coefficient（r^2） was 1.000. The relative standard deviationof sample detection results was 1.31%. The detection results of the method had no significant difference compared withtraditional visible spectrophotometry by t-Test and F-test. The method can be used for determining relative molecularmass and its distribution simultaneously,and controlling the quality of the retention test standard materials （PEGs）.