Im Kyuhyun, Park Hae-Woong, Lee Sekyung, Chang Taihyun
Department of Chemistry and BK 21 School of Molecular Science, Pohang University of Science and Technology, Nam-Gu, Pohang, South Korea.
J Chromatogr A. 2009 May 22;1216(21):4606-10. doi: 10.1016/j.chroma.2009.03.072. Epub 2009 Apr 1.
In recent years, two-dimensional liquid chromatography (2D-LC) has been used increasingly for the analysis of synthetic polymers. A 2D-LC analysis provides richer information than a single chromatography analysis at the cost of longer analysis time. The time required for a comprehensive 2D-LC analysis is essentially proportional to the analysis time of the second dimension separation. Many of 2D-LC analyses of synthetic polymers have employed size exclusion chromatography (SEC) for the second-dimension analysis due to the relatively short analysis time in addition to the wide use in the polymer analysis. Nonetheless, short SEC columns are often used for 2D-LC analyses to reduce the separation time, which inevitably deteriorates the resolution. In this study, we demonstrated that high temperature SEC can be employed as an efficient second-LC in the 2D-LC separation of synthetic polymers. By virtue of high temperature operation (low solvent viscosity and high diffusivity of the polymer molecules), a normal length SEC column can be used at high flow rate with little loss in resolution.
近年来,二维液相色谱(2D-LC)越来越多地用于合成聚合物的分析。二维液相色谱分析以更长的分析时间为代价,提供比单一色谱分析更丰富的信息。全面二维液相色谱分析所需的时间基本上与第二维分离的分析时间成正比。由于分析时间相对较短且在聚合物分析中广泛应用,许多合成聚合物的二维液相色谱分析都采用尺寸排阻色谱(SEC)进行第二维分析。尽管如此,短的SEC柱常用于二维液相色谱分析以减少分离时间,这不可避免地会降低分离度。在本研究中,我们证明了高温SEC可作为合成聚合物二维液相色谱分离中高效的第二维液相色谱。由于高温操作(低溶剂粘度和聚合物分子的高扩散率),正常长度的SEC柱可在高流速下使用,而分离度几乎没有损失。