Bruchet Anthony, Dugas Vincent, Mariet Clarisse, Goutelard Florence, Randon Jérôme
Commissariat à l'Energie Atomique, Saclay, DEN/DPC/SECR/LANIE, Gif-sur-Yvette, France; Laboratoire des Sciences Analytiques (UMR CNRS 5180), Université de Lyon, Villeurbanne, France.
J Sep Sci. 2011 Aug;34(16-17):2079-87. doi: 10.1002/jssc.201100180. Epub 2011 May 27.
An efficient and reproducible photopolymerized poly(glycidyl methacrylate-co-ethylene dimethacrylate) was synthesized in Teflon-coated fused-silica capillaries (100 μm id) and functionalized by reaction of triethylamine with reactive epoxy groups. We report here the successful transfer of a standard polymerization mixture optimized for the thermally initiated synthesis of glycidyl-based monolith to photo-induced polymerization. The monolith obtained after optimization of the photo-initiation conditions was characterized in reverse-phase chromatography evaluating its suitability in terms of efficiency, retention and hydrodynamic permeability. Reproducibility of the photo-induced procedure was satisfactory with RSD below 6% for retention and efficiency and slightly higher for hydrodynamic permeability (12%). The functionalized generic support was then used in nano-ion-exchange chromatography. Efficiencies up to 75,000 plates/m, ion-exchange capacity of 8 nano-equivalents/cm of monolithic column, with a combination of a satisfactory hydrodynamic permeability allowed to perform fast separations of five inorganic anions in <3 min maintaining baseline resolution. The efficiency of the monolith was not retention-dependent, demonstrating its wide range of possible applications for highly retained anions.
在涂有特氟龙的熔融石英毛细管（内径100μm）中合成了一种高效且可重现的光聚合聚（甲基丙烯酸缩水甘油酯-共-二甲基丙烯酸乙二醇酯），并通过三乙胺与活性环氧基团的反应进行功能化。我们在此报告了将针对热引发合成缩水甘油基整体柱优化的标准聚合混合物成功转移至光引发聚合的过程。在反相色谱中对优化光引发条件后获得的整体柱进行了表征，评估了其在效率、保留和流体动力学渗透率方面的适用性。光引发过程的重现性令人满意，保留率和效率的相对标准偏差（RSD）低于6%，流体动力学渗透率的RSD略高（12%）。然后将功能化的通用载体用于纳米离子交换色谱。效率高达75000塔板/米，整体柱的离子交换容量为8纳当量/厘米，结合令人满意的流体动力学渗透率，能够在不到3分钟的时间内对五种无机阴离子进行快速分离，并保持基线分辨率。整体柱的效率不依赖于保留率，这表明其在高保留阴离子方面具有广泛的潜在应用。
