Ultrahigh pressure reversed-phase liquid chromatography in packed capillary columns
Ultrahigh pressure reversed-phase liquid chromatography in packed capillary columns
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DOI：
10.1021/ac961094r
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发表时间：
1997-03-15
影响因子：
7.4
通讯作者：
Jorgenson, JW
中科院分区：
文献类型：
--
作者：
MacNair, JE;Lewis, KC;Jorgenson, JW
在液相色谱中使用极高的压力可以提高效率并减少填充有小颗粒的柱的分析时间。在这项工作中，熔融石英毛细管内径为30 μ m的浆料填充1.5 μ m无孔十八烷基硅烷改性的二氧化硅颗粒。这些色谱柱的长度可达66 cm，填充压力高达4100 bar（60 000 psi）。在最佳流速附近，色谱柱对轻度保留的化合物（k' < 0.5）产生多达300 000个理论塔板，对更多保留的化合物（k'接近2）产生超过200 000个理论塔板。这些转化为低至2.1 μ m的板高度（H-min）。在最佳流速下运行所需的压力大约为1400巴（20 000 psi）。在这些压力下的分析时间约为30分钟（k'近似为2），并且在高于最佳流速的情况下可以减少到小于10分钟。观察到容量因子随施加的压力线性增加。
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 mu m are slurry packed with 1.5 mu m 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 now 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' approximate to 2). These translate to plate heights (H-min) as low as 2.1 mu m. 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' approximate to 2) and can be reduced to less than 10 min at higher than optimum now rates, Capacity factors are observed to increase linearly with applied pressure.