High-Efficiency Liquid Chromatographic Separation Utilizing Long Monolithic Silica Capillary Columns
High-Efficiency Liquid Chromatographic Separation Utilizing Long Monolithic Silica Capillary Columns
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DOI：
10.1021/ac801042c
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发表时间：
2008-11-15
影响因子：
7.4
通讯作者：
Tanaka, Nobuo
中科院分区：
文献类型：
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作者：
Miyamoto, Kosuke;Hara, Takeshi;Tanaka, Nobuo
制备100μmW的长整体硅胶-C-18毛细管柱，并在高达47MPa的压力下使用反相HPLC检查柱效。在 1-2 mm/s 的线速度下，使用乙腈-水 (80/20) 流动相、柱死时间 (t(0)) 为 5-40 分钟，单根色谱柱（长度 90-440 cm）可产生 100000-500000 个理论塔板。可以制备最小板高度为8.5+/-0.5μm、渗透率为(1.45+/-0.09)×10(-13)m(2)的柱。通过芳香烃、苯衍生物和蛋白质消化物的高效分离，证明了长十八烷基硅烷化整体式硅胶毛细管柱的色谱性能。注射量高达 0.5-2 ng 时仍能保持肽的效率。当三个内径100μm的将色谱柱连接起来形成1130-1240 cm的色谱柱系统，生成了1000000个芳烃理论塔板，保留因子高达2.4，t(0)为150 min。保留溶质获得了非常高的效率这一事实表明了这些长整体式二氧化硅毛细管柱的实际用途。
Long monolithic silica-C-18 capillary columns of 100 mu m W. were prepared, and the efficiency was examined using reversed-phase HPLC under a pressure of up to 47 MPa. At linear velocities of 1-2 mm/s, 100000-500000 theoretical plates could be generated with a single column (90-440 cm in length) using an acetonitrile-water (80/20) mobile phase with a column dead time (t(0)) of 5-40 min. It was possible to prepare columns with a minimum plate height of 8.5 +/- 0.5 mu m and permeability of (1.45 +/- 0.09) X 10(-13) m(2). The chromatographic performance of a long octadecylsilylated monolithic silica capillary column was demonstrated by the high-efficiency separations of aromatic hydrocarbons, benzene derivatives, and a protein digest. The efficiency for a peptide was maintained for an injection of up to 0.5-2 ng. When three 100 mu m i.d. columns were connected to form a 1130-1240 cm column system, 1000000 theoretical plates were generated for aromatic hydrocarbons with retention factors of up to 2.4 with a t(0) of 150 min. The fact that very high efficiencies were obtained for the retained solutes suggests the practical utility of these long monolithic silica capillary columns.