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首页> 外文期刊>Journal of liquid chromatography and related technologies >Preparation of Poly(1-dodecene-co-trimethylol propane triacrylate-co-ethylene dimethacrylate) Monolithic Column for HPLC Separations of Small Molecules
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Preparation of Poly(1-dodecene-co-trimethylol propane triacrylate-co-ethylene dimethacrylate) Monolithic Column for HPLC Separations of Small Molecules

机译:聚(1-十二碳烯-三羟甲基丙烷三丙烯酸酯-二甲基丙烯酸乙烯酯)整体柱的制备

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摘要

A new poly(1-dodecene-co-trimethylol propane triacrylate-co-ethylene dimethacrylate) [poly(C12-co-TMPTA-co-EDMA)] monolithic column was prepared via in situ free-radical polymerization reaction. Various parameters affecting the polymerization were investigated and optimized. The permeability of the monolithic column was calculated as 2.9098x10(-14)m(2) with methanol as the mobile phase and the surface areas was 73.1m(2)/g by the nitrogen adsorption-desorption experiment. The morphologies of the monolith were characterized by scanning electron microscopy (SEM) and the mechanical strength has been studied in detail as well. The prepared monolith was then used as the stationary phase of reversed phase high-performance liquid chromatography (RP-HPLC) to separate small molecule compounds. Column efficiency for chlorobenzene reached 14,340 theoretical plates per meter. The monolith also showed satisfactory reproducibility, based on the retention times of benzene, phenol, chlorobenzene, diphenylamine, and anthracene; the relative standard deviation (RSD) values for run-to-run, column-to-column and batch-to-batch were less than 0.62%, 3.2%, and 5.7%, respectively.
机译:通过原位自由基聚合反应制备了一种新型的聚(1-十二碳烯-三羟甲基丙烷三丙烯酸酯-二甲基丙烯酸乙二酯)[整体(C12-co-TMPTA-co-EDMA)]整体柱。研究和优化了影响聚合的各种参数。用氮气作为流动相,整体柱的渗透率计算为2.9098x10(-14)m(2),通过氮吸附-脱附实验得到的表面积为73.1m(2)/ g。整体结构的形貌通过扫描电子显微镜(SEM)进行了表征,并且还对机械强度进行了详细研究。然后将制得的整料用作反相高效液相色谱(RP-HPLC)的固定相,以分离小分子化合物。氯苯的柱效达到每米14,340个理论塔板数。基于苯,苯酚,氯苯,二苯胺和蒽的保留时间,整料还显示出令人满意的重现性;批次间,柱间和批次之间的相对标准偏差(RSD)值分别小于0.62%,3.2%和5.7%。

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