High-Efficiency Liquid Chromatographic Separation Utilizing Long Monolithic Silica Capillary Columns

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• 作者：Kosuke Miyamoto ; Takeshi Hara ; Hiroshi Kobayashi ; Hironobu Morisaka ; Daisuke Tokuda ; Kanta Horie ; Kodai Koduki ; Satoshi Makino ; Oscar Nú ; ñ ; ez ; Chun Yang ; Takefumi Kawabe ; Tohru Ikegami ; Hiro
• 刊名：Analytical Chemistry
• 出版年：2008
• 出版时间：November 15, 2008
• 年：2008
• 卷：80
• 期：22
• 页码：8741-8750
• 全文大小：336K
• 年卷期：v.80,no.22(November 15, 2008)
• ISSN：1520-6882

文摘

Long monolithic silica-C₁₈ capillary columns of 100 μm i.d. 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 (t₀) of 5−40 min. It was possible to prepare columns with a minimum plate height of 8.5 ± 0.5 μm and permeability of (1.45 ± 0.09) × 10⁻¹³ m². 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 μm 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 t₀ 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.