Department of Analytical Chemistry, Faculty of Chemistry, University of Valencia, 46100 Valencia, Spain.
J Chromatogr A. 2010 May 7;1217(19):3231-7. doi: 10.1016/j.chroma.2009.08.075. Epub 2009 Sep 1.
The synthesis of lauryl methacrylate monoliths for capillary electrochromatography by UV polymerization using several free-radical initiators (alpha,alpha'-azobisisobutyronitrile, 2,2-dimethoxy-2-phenylacetophenone, dibenzoyl peroxide (BPO) and lauroyl peroxide (LPO)) has been investigated. Using a 1,4-butanediol/1-propanol mixture as porogenic solvent, the influence of each initiator and its content on the morphological and electrochromatographical properties of beds was evaluated. Under their respective optimum content, satisfactory separations of a test mixture of PAHs with similar efficiencies (minimum plate heights of 8.0-12.7 microm obtained from Van Deemter plots) were achieved for the four investigated photo-initiators. The columns photo-polymerized with LPO provided the best compromise between chromatographic performance and analysis time. Moreover, this initiator showed a fine control in the column retention properties. The resulting monolithic columns exhibited a good run-to-run repeatability in the tested chromatographic parameters (RSD<2.4%) for all initiators investigated; and satisfactory column-to-column repeatability (RSD<6.0%), except for beds photo-polymerized with BPO (RSD<10.8%).
通过使用几种自由基引发剂（α，α'-偶氮二异丁腈、2,2-二甲氧基-2-苯乙酮、过氧化二苯甲酰（BPO）和过氧化月桂酰（LPO））的紫外光聚合，合成了用于毛细管电色谱的月桂基甲基丙烯酸酯整体柱。使用 1,4-丁二醇/1-丙醇混合物作为致孔溶剂，评估了每种引发剂及其含量对床的形态和电色谱性能的影响。在各自的最佳含量下，四种被研究的光引发剂都实现了对具有相似效率的 PAHs 测试混合物的令人满意的分离（从 Van Deemter 图中获得的最小板高为 8.0-12.7 µm）。用 LPO 光聚合的柱子在色谱性能和分析时间之间取得了最佳的折衷。此外，该引发剂对柱保留性能具有精细的控制。所得到的整体柱在所有被研究的色谱参数（RSD<2.4%）中表现出良好的运行重复性；除了用 BPO 光聚合的床（RSD<10.8%）外，柱间重复性也令人满意（RSD<6.0%）。
