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A novel ionic liquid-based monolithic column and its application in the efficient separation of proteins and small molecules by high-performance liquid chromatography

机译:新型离子液体整体柱及其在高效液相色谱法有效分离蛋白质和小分子中的应用

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摘要

A novel skeleton porous polymer-based monolith chromatography column has successfully been prepared using an in situ free radical polymerization technique. A 50 mm x 4.6 mm i.d. stainless steel chromatographic column used dodecanol as porogen and ionic liquid (IL), 1-dodecene (C12) and trimethylol propane triacrylate (TMPTA) as monomers, and ethylene dimethacrylate as crosslinker. The effect of variables such as temperature and porogen solvent content on the porous structure was studied in detail. The polymer-based monolith obtained was characterized by scanning electron microscopy, infrared spectroscopy, mercury intrusion porosimetry, and nitrogen adsorption. The results indicated that the monolithic column had a porous structure, good mechanical stability, high permeability (6.77 x 10(-14) m(2)), and a high specific surface area (155.62 m(2) g(-1)). The liquid chromatographic performance of the monolith was evaluated in the separation of lysozyme from egg white and in the separation of a variety of mixtures of small molecules, such as amines and benzene analogues. The column showed good repeatability and reproducibility, and the column-to-column (n = 7) and batch-to-batch (n = 5) reproducibility was 2.85 and 3.15%, respectively.
机译:使用原位自由基聚合技术已成功制备了新型的基于骨架多孔聚合物的整体式色谱柱。内径50毫米x 4.6毫米不锈钢色谱柱使用十二烷醇作为致孔剂和离子液体(IL),1-十二烯(C12)和三羟甲基丙烷三丙烯酸酯(TMPTA)作为单体,以及二甲基丙烯酸乙二酯作为交联剂。详细研究了温度和致孔剂溶剂含量等变量对多孔结构的影响。通过扫描电子显微镜,红外光谱,压汞法和氮吸附来表征所获得的基于聚合物的整料。结果表明,整体柱具有多孔结构,良好的机械稳定性,高渗透性(6.77 x 10(-14)m(2))和高比表面积(155.62 m(2)g(-1)) 。在从蛋清中分离溶菌酶和分离各种小分子混合物(例如胺和苯类似物)的过程中,对整料的液相色谱性能进行了评估。色谱柱显示出良好的可重复性和可重复性,色谱柱间(n = 7)和批次间(n = 5)的重现性分别为2.85和3.15%。

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