Development of monolithic silica columns in capillary for high-speed and high-performance HPLC

本文研究了多孔硅胶整体柱在毛细管中的应用，以获得比颗粒填充柱更高的性能。进行了以下实验。(1)用烷氧基硅烷在毛细管中制备硅胶整体柱。(2)在25-250 μm各种尺寸的毛细管中制备整体硅胶柱。(3)研究了微区尺寸（通孔尺寸+二氧化硅骨架尺寸）和通孔尺寸与骨架尺寸之比对性能的影响。(4)高效硅胶整体柱的制备。(5)短时间内制备高效硅胶整体柱。(6)硅胶整体柱谱带增宽影响因素的研究。(7)微型HPLC和CEC中硅胶整体柱的评价。(8)本文介绍了硅胶整体柱在碱、可离解化合物和烃类等多种化合物分离中的应用。 ...更多信息 保持。(1)在直径为50-250 μm的熔融石英毛细管中，可以制备出附着在管壁上的网络型整体石英。(2)在颗粒填充柱中，微区尺寸的减小表现出与颗粒尺寸的减小类似的效果，导致更高的柱压降和更高的柱效率。(3)100 μm，250 cm的硅胶毛细管柱，t0 = 1000 s，理论塔板数为200，000 ~ 300，000. (4)采用通孔为1.5 μm、骨架尺寸为0.8 μm的硅胶毛细管整体柱，理论塔板数为10.000，t0 = 15 S。(5)硅胶整体柱的谱带展宽主要是由A项或移动的相缓慢传质的贡献所决定的，特别是当硅胶整体柱具有较大的通孔尺寸时。具有小畴尺寸的整料显示固定相传质的主要贡献。(6)混合型硅胶整体柱对碱、β-受体阻滞剂、甾体、酮类、邻苯二甲酸酯类、醇类和烃类等多种化合物具有良好的分离性能，200 μm毛细管硅胶整体柱在常规条件下的分离性能是颗粒填充柱的2 ~ 3倍，且使用方便。它们可用于分离多种化合物。因此，它们接近实际使用。(1)大口径毛细管的制备、柱上反应的各种表面单官能化、微区结构的优化、硅胶整体柱谱带展宽的理论和实验研究等将是该领域的基础性和实用性课题。其他研究将包括在芯片通道中制备整体二氧化硅和在微型HPLC中进行多维色谱。少

The development of porous monolithic silica columns in capillary for micro-HPLC was studied to achieve higher performance than columns packed with particles. Following experiments were carried out.(1) Preparation of a monolithic silica column in a capillary from alkoxysilanes.(2) Preparation of monolithic silica columns in capillaries of various sizes, 25-250 μm.(3) Study on the effect of domain size (through-pore size + silica skeleton size) and the ratio between through-pore size and skeleton size on the performance.(4) Preparation of ultrahigh efficiency monolithic silica columns.(5) Preparation of monolithic silica columns showing high efficiency in a short time.(6) Study on the factors determining band-broadening in a monolithic silica column.(7) Evaluation of monolithic silica columns in micro-HPLC and CEC.(8) Application of monolithic silica columns for the separation of various types of compounds including bases, dissociable compounds, and hydrocarbons.Following results were ob … More tained.(1) It is possible to prepare network-type monolithic silica attached to the tube wall of fused silica capillary having 50-250 μm diameter.(2) Decrease in domain size showed similar effects as the decrease in particle size in a particle-packed column, causeing higher column pressure drop and higher column efficiency.(3) A monolithic silica capillary column of 100 μm, 250 cm gave 200, 000 - 300, 000 theoretical plates with to = 1000 s.(4) A monolithic silica capillary column with through-pores = 1.5 μm and skeleton size 0.8 μm gave 10.000 theoretical plates with to = 15 S.(5) The band-broadening in a monolithic silica column is dominated by A-term, or the contrubution of slow mass transfer in mobile phase, especially when the monolith possesses large through-pore size. Monoliths having small domain size showed the major contibution of stationary phase mass transfer.(6) Hybrid-type monolithic silica columns showed high performance for the separation of various types of compounds including bases, b-blockers, steroids, ketones, phthalates, aicohols, and hydrocarbon of various structures.Monolithic silica columns in 200 μm capillary can show performance 2 - 3 times higher than particle-packed columns under common conditions and are relatively easy to use. They can be applied for the separatin of a wide range of compounds. Thus they are close to practical use. (1) Preparation of larger-sized capillary, (2) various surface monofication by on-column reactions(3) optimization of domain structures, and (4) theoretical and experimental study on band-broadening in monolithic silica columns will be practical and basic subjects to study in this area. Other study will include the preparation of monolithic silica in a chip channels and multidimensional chromatography in a microscale HPLC. Less