Monolithic silica columns for high-efficiency separations by high-performance liquid chromatography
Monolithic silica columns for high-efficiency separations by high-performance liquid chromatography
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DOI：
10.1016/s0021-9673(01)01580-1
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发表时间：
2002-06-25
影响因子：
4.1
通讯作者：
Tanaka, N
中科院分区：
文献类型：
--
作者：
Ishizuka, N;Kobayashi, H;Tanaka, N
尝试用毛细管高效液相色谱法生成大量理论板。采用溶胶-凝胶法制备了骨架小（约2 μ m）、通孔大（约8 μ m）的硅胶整体柱，柱上反应衍生为C-18相。高外部孔隙度（>80%）和大通孔导致高渗透率(K = 1.2 X 10（-12) m(2)）。毛细管中硅胶整体柱在80%乙腈中以1 mm/s的线速度产生约12 μ m的板高。分离阻抗，E值，被发现低至200，这是大约一个数量级低于报告值的传统柱填充5个mum颗粒。在柱效率和压降方面，制备的重现性在15%以内。在非常低的压力下，使用130厘米的柱可以产生100,000个板(
Generation of a large number of theoretical plates was attempted by capillary HPLC. Monolithic silica columns having small skeletons (ca. 2 mum) and large through-pores (ca. 8 mum) were prepared by a sol-gel method in a fused-silica capillary (50 mum I.D.), and derivatized to C-18 phase by on-column reaction. High external porosity (>80%) and large through-pores resulted in high permeability (K = 1.2 X 10(-12) m(2)). The monolithic silica column in the capillary produced a plate height of about 12 mum in 80% acetonitrile at a linear velocity of 1 mm/s. Separation impedance, E value, was found to be as low as 200, that was about an order of magnitude lower than reported values for conventional columns packed with 5 mum particles. Reproducibility of preparation within 15% was obtained for column efficiency and for pressure drop. It was possible to generate 100,000 plates by using a 130-cm column at very low pressure (