Key Laboratory of Pharmaceutical Quality Control of Hebei Province, College of Pharmaceutical Sciences, Hebei University, Baoding 071002, China.
J Chromatogr A. 2013 Jul 5;1297:131-7. doi: 10.1016/j.chroma.2013.04.076. Epub 2013 May 3.
A new polymeric monolith was synthesized in fused-silica capillary by in situ polymerization technique. In the polymerization, bisphenol A epoxy vinyl ester resin (VER) was used as the functional monomer, ethylene glycol dimethacrylate (EDMA) as the crosslinking monomer, 1,4-butanediol, 1-propanol and water as the co-porogens, and azobisisobutyronitrile (AIBN) as the initiator. The conditions of polymerization have been optimized. Morphology of the prepared poly (VER-co-EDMA) monolith was investigated by the scanning electron microscopy (SEM); pore properties were assayed by mercury porosimetry and nitrogen adsorption. The optimized poly (VER-co-EDMA) monolith showed a uniform structure, good permeability and mechanical stability. Then, the column was used as the stationary phase of high performance liquid chromatography (HPLC) to separate the mixture of benzene derivatives. The best column efficiency achieved for phenol was 235790 theoretical plates per meter. Baseline separations of benzene derivatives and halogenated benzene compounds under optimized isocratic mode conditions were achieved with high column efficiency. The column showed good reproducibility: the relative standard deviation (RSD) values based on the retention times (n=3) for run-to-run, column-to-column and batch-to-batch were less than 0.98, 1.68, 5.48%, respectively. Compared with poly (BMA-co-EDMA) monolithic column, the proposed monolith exhibited more efficiency in the separation of small molecules.
一种新型聚合整体柱通过原位聚合法在熔融石英毛细管中合成。在聚合过程中,双酚 A 环氧乙烯基酯树脂(VER)用作功能单体,乙二醇二甲基丙烯酸酯(EDMA)用作交联单体,1,4-丁二醇、1-丙醇和水作为共致孔剂,偶氮二异丁腈(AIBN)作为引发剂。优化了聚合条件。通过扫描电子显微镜(SEM)研究了制备的聚(VER-co-EDMA)整体柱的形貌;通过压汞法和氮气吸附法测定了孔性能。优化后的聚(VER-co-EDMA)整体柱具有均匀的结构、良好的渗透性和机械稳定性。然后,该柱作为高效液相色谱(HPLC)的固定相用于分离苯衍生物混合物。酚的最佳柱效达到 235790 理论板/米。在优化的等度模式条件下,苯衍生物和卤代苯化合物实现了基线分离,柱效较高。该柱具有良好的重现性:基于保留时间(n=3)的相对标准偏差(RSD)值分别小于 0.98、1.68 和 5.48%。与聚(BMA-co-EDMA)整体柱相比,该整体柱在小分子分离方面表现出更高的效率。