MacNair J E, Lewis K C, Jorgenson J W
Department of Chemistry, University of North Carolina at Chapel Hill 27599-3290, USA.
Anal Chem. 1997 Mar 15;69(6):983-9. doi: 10.1021/ac961094r.
The use of extremely high pressures in liquid chromatography can improve the efficiency and reduce analysis time for columns packed with small particles. In this work, fused-silica capillaries with inner diameters of 30 microns are slurry packed with 1.5 microns nonporous octadecylsilane-modified silica particles. These columns are prepared in lengths up to 66 cm with packing pressures as high as 4100 bar (60,000 psi). Near the optimum flow rate, columns generate as many as 300,000 theoretical plates for lightly retained compounds (k' < 0.5) and over 200,000 plates for more retained compounds (k' approximately 2). These translate to plate heights (Hmin) as low as 2.1 microns. The pressures required to run at optimum flow rates are on the order of 1400 bar (20,000 psi). Analysis times at these pressures are on the order of 30 min (k' approximately 2) and can be reduced to less than 10 min at higher than optimum flow rates. Capacity factors are observed to increase linearly with applied pressure.
在液相色谱中使用极高的压力可以提高装填有小颗粒的色谱柱的效率并缩短分析时间。在这项工作中，内径为30微米的熔融石英毛细管被用1.5微米无孔十八烷基硅烷改性硅胶颗粒进行匀浆装填。这些色谱柱的制备长度可达66厘米，装填压力高达4100巴（60,000磅力/平方英寸）。在接近最佳流速时，对于保留较弱的化合物（k' < 0.5），色谱柱可产生多达300,000个理论塔板，对于保留较强的化合物（k'约为2），则可产生超过200,000个塔板。这相当于塔板高度（Hmin）低至2.1微米。以最佳流速运行所需的压力约为1400巴（20,000磅力/平方英寸）。在这些压力下的分析时间约为30分钟（k'约为2），在高于最佳流速时可缩短至不到10分钟。观察到容量因子随施加压力呈线性增加。
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