Monolithic silica columns with various skeleton sizes and through-pore sizes for capillary liquid chromatography
Monolithic silica columns with various skeleton sizes and through-pore sizes for capillary liquid chromatography
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DOI：
10.1016/s0021-9673(02)00133-4
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发表时间：
2002-06-28
影响因子：
4.1
通讯作者：
Tanaka, N
中科院分区：
文献类型：
--
作者：
Motokawa, M;Kobayashi, H;Tanaka, N
试图减小整体硅胶柱的通孔尺寸和骨架尺寸以在短时间内提供高分离效率。在熔融石英毛细管（50-200 μ m I.D.）中制备具有各种尺寸的骨架（类似于1 -2 μ m）和通孔（类似于2 -8 μ m）的整体式二氧化硅柱。衍生化至C-18相后，在HPLC中评价色谱柱。可以在内径高达200 μ m的毛细管中制备单片二氧化硅结构。由四甲氧基硅烷和甲基三甲氧基硅烷的混合物制得。正如预期的那样，具有较小域尺寸的整体硅胶柱显示出更高的柱效率和更高的压降。高的外孔隙度（>80%）和大的通孔导致高的渗透率（K=8.10（-14）-1.3（.）10（-12）m（2）），比填充有5 μ m二氧化硅颗粒的柱高2-30倍。在毛细管中制备的整体式二氧化硅柱产生约8-12 μ m的板高，具有80%乙腈水溶液移动的相，线速度为1 mm/s。分离阻抗，E，被认为是低至100在最佳条件下，一个值约一个数量级低于传统的列与5微米颗粒填充。虽然具有较小畴尺寸的柱通常导致较高的分离阻抗和较低的总性能，但整体硅胶柱在压力驱动条件下显示出超出常规颗粒填充柱的极限的性能。(C)2002 Elsevier Science BV保留所有权利。
Reduction of through-pore size and skeleton size of a monolithic silica column was attempted to provide high separation efficiency in a short time. Monolithic silica columns were prepared to have various sizes of skeletons (similar to1-2 mum) and through-pores (similar to2-8 mum) in a fused-silica capillary (50-200 mum I.D.). The columns were evaluated in HPLC after derivatization to C-18 phase. It was possible to prepare monolithic silica structures in capillaries of up to 200 mum I.D. from a mixture of tetramethoxysilane and methyltrimethoxysilane. As expected, a monolithic silica column with smaller domain size showed higher column efficiency and higher pressure drop. High external porosity (>80%) and large through-pores resulted in high permeability (K=8.10(-14) -1.3(.)10(-12) m(2)) that was 2-30 times higher than that of a column packed with 5-mum silica particles. The monolithic silica columns prepared in capillaries produced a plate height of about 8-12 mum with an 80% aqueous acetonitrile mobile phase at a linear velocity of 1 mm/s. Separation impedance, E, was found to be as low as 100 under optimum conditions, a value about an order of magnitude lower than reported for conventional columns packed with 5-mum particles. Although a column with smaller domain size generally resulted in higher separation impedance and the lower total performance, the monolithic silica columns showed performance beyond the limit of conventional particle-packed columns under pressure-driven conditions. (C) 2002 Elsevier Science BV All rights reserved.