Institute of Pharmaceutical Sciences, Pharmaceutical (Bio-)Analysis, University of Tübingen, Tübingen, Germany.
Center for Light-Matter Interaction, Sensors & Analytics (LISA+), University of Tübingen, Tübingen, Germany.
Electrophoresis. 2019 Dec;40(23-24):3132-3139. doi: 10.1002/elps.201900316. Epub 2019 Oct 15.
The successful fabrication of monolithic capillary columns for enantiomer separations was achieved within vinylized fused silica capillaries via fast "one-pot" photo-initiated free radical polymerization reaction. A mixture consisting of polyhedral oligomeric silsesquioxane, O-[2-(methacryloyloxy)ethylcarbamoyl]-10,11-dihydroquinidine was copolymerized in the presence of n-butanol, ethylene glycol and photo-initiator 2,2-dimethoxy-2-phenylacetophenone. The morphology of the resultant polymeric hybrid inorganic-organic material and its permeability as well as porosity can be controlled by adjusting the composition of the monomers and binary porogenic solvent. The chromatographic characteristics of the columns have been investigated. Separation factors of N-acetyl-phenylalanine (Ac-Phe) and dichlorprop dropped with decrease of chiral functional monomer. Permeability was better when the macroporogen ethyleneglycol was present at higher concentrations during the polymerization. In general, the chiral compounds were well separated (dichlorprop: α = 1.53, R up to 4.14; Ac-Phe: α = 1.36, R up to 2.69) by nano-HPLC with an optimized enantioselective monolithic capillary column which can be prepared within a few minutes.
通过快速的“一锅法”光引发自由基聚合反应，在乙烯基化熔融石英毛细管内成功制备了用于对映体分离的整体式毛细管柱。多面体低聚倍半硅氧烷、O-[2-（甲基丙烯酰氧基）乙基]碳酰-10,11-二氢奎宁与正丁醇、乙二醇和光引发剂 2,2-二甲氧基-2-苯乙酮共聚。通过调整单体和二元致孔溶剂的组成，可以控制所得聚合的无机-有机杂化材料的形态及其渗透性和孔隙率。考察了柱的色谱特性。N-乙酰苯丙氨酸（Ac-Phe）和二氯丙的分离因子随着手性功能单体的减少而降低。在聚合过程中，当大分子致孔剂乙二醇的浓度较高时，渗透性更好。一般来说，通过优化的手性纳诺高效液相色谱可以很好地分离手性化合物（二氯丙：α=1.53，R 最高可达 4.14；Ac-Phe：α=1.36，R 最高可达 2.69），而这种手性整体式毛细管柱可以在几分钟内制备。
