Lämmerhofer M, Peters E C, Yu C, Svec F, Fréchet J M
Department of Chemistry, University of California, Berkeley 94720-1460, USA.
Anal Chem. 2000 Oct 1;72(19):4614-22. doi: 10.1021/ac000322l.
Monolithic columns for chiral capillary electrochromatography have been prepared within the confines of untreated fused-silica capillaries in a single step by a simple copolymerization of mixtures of O-[2-(methacryloyloxy)ethylcarbamoyl]-10,11-dihydroquinidine , ethylene dimethacrylate, and glycidyl methacrylate or 2-hydroxyethyl methacrylate in the presence of mixture of cyclohexanol and 1-dodecanol as a porogenic solvent. The porous properties of the monolithic columns can easily be controlled through changes in the composition of the binary porogenic solvent. Although both thermal- and UV light-initiated polymerizations afford useful capillary columns, monoliths prepared using the former approach exhibit better chromatographic properties. The ability to control pore size independently of the polymerization mixture composition enables the preparation of monoliths with varying percentages of the chiral monomer and cross-linker, as well as the optimization of their separation properties. Very good separations of model racemate (R,S)-N-3,5-dinitrobenzoylleucine were achieved using an optimized monolithic CEC column, with high efficiencies of up to 74000 plates/m for the retained peaks.
用于手性毛细管电色谱的整体柱是在未处理的熔融石英毛细管内,通过O-[2-(甲基丙烯酰氧基)乙基氨基甲酰基]-10,11-二氢奎尼丁、二甲基丙烯酸乙烯酯和甲基丙烯酸缩水甘油酯或甲基丙烯酸2-羟乙酯的混合物,在作为致孔溶剂的环己醇和1-十二醇混合物存在下,一步简单共聚制备而成。整体柱的多孔性质可通过改变二元致孔溶剂的组成轻松控制。尽管热引发聚合和紫外光引发聚合都能得到有用的毛细管柱,但采用前一种方法制备的整体柱表现出更好的色谱性能。独立于聚合混合物组成控制孔径的能力使得能够制备具有不同手性单体和交联剂百分比的整体柱,并优化其分离性能。使用优化的整体式CEC柱对模型外消旋体(R,S)-N-3,5-二硝基苯甲酰亮氨酸实现了非常好的分离,保留峰的效率高达74000塔板/米。