Aydoğan Cemil
Bingöl University, Department of Food Engineering, 12000 Bingöl, Turkey.
J Chromatogr A. 2015 May 1;1392:63-8. doi: 10.1016/j.chroma.2015.03.014. Epub 2015 Mar 14.
In this study, an anion-exchange/hydrophobic polymethacrylate-based stationary phase was prepared for nano-liquid chromatography of small organic molecules and inorganic anions. The stationary phase was synthesized by in situ polymerization of 3-chloro-2-hydroxypropylmethacrylate and ethylene dimethacrylate inside silanized 100 μm i.d. fused silica capillary. The porogen mixture consisted of toluene and dodecanol. The pore size distrubution profiles of the resulting monolith were determined by mercury intrusion porosimetry and the morphology of the prepared monolith was investigated by scanning electron microscope. Good permeability, stability and column efficiency were observed on the monolithic column with nano flow. The produced monolithic column, which contains reactive chloro groups, was then modified by reaction with N,N-dimethyl-N-dodecylamine to obtain an anion-exchange/hydrophobic monolithic stationary phase. The functionalized monolith contained ionizable amine groups and hydrophobic groups that are useful of anion-exchange/hydrophobic mixed-mode chromatography. The final monolithic column performance with respect to anion-exchange and hydrophobic interactions was assesed by the separation of alkylbenzene derivatives, phenolic compounds and inorganic anions, respectively. Theoretical plate numbers up to 23,000 plates/m were successfully achieved in the separation of inorganic anions.
在本研究中,制备了一种基于阴离子交换/疏水聚甲基丙烯酸酯的固定相,用于小分子有机化合物和无机阴离子的纳米液相色谱分析。该固定相通过在硅烷化的内径为100μm的熔融石英毛细管内原位聚合甲基丙烯酸3-氯-2-羟丙酯和二甲基丙烯酸乙二酯合成。致孔剂混合物由甲苯和十二烷醇组成。通过压汞法测定所得整体柱的孔径分布曲线,并通过扫描电子显微镜研究制备的整体柱的形态。在纳流条件下,整体柱表现出良好的渗透性、稳定性和柱效。然后,将含有反应性氯基团的制备好的整体柱与N,N-二甲基-N-十二烷基胺反应进行改性,以获得阴离子交换/疏水整体固定相。功能化整体柱含有可离子化的胺基和疏水基团,可用于阴离子交换/疏水混合模式色谱分析。分别通过分离烷基苯衍生物、酚类化合物和无机阴离子来评估最终整体柱在阴离子交换和疏水相互作用方面的性能。在无机阴离子的分离中成功实现了高达23,000塔板数/米的理论塔板数。