Monolithic silica rod columns for high-efficiency reversed-phase liquid chromatography
Monolithic silica rod columns for high-efficiency reversed-phase liquid chromatography
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DOI：
10.1016/j.chroma.2010.11.032
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发表时间：
2011-04-15
影响因子：
4.1
通讯作者：
Tanaka, Nobuo
中科院分区：
文献类型：
--
作者：
Miyazaki, Shota;Takahashi, Masakazu;Tanaka, Nobuo
对新型整体硅胶棒柱的色谱性能进行了检测。用于该研究的二氧化硅棒柱由四甲氧基硅烷制备，用十八烷基甲硅烷基部分改性，并封装在不锈钢保护柱中，二氧化硅和不锈钢管之间有两个聚合物层。 25 cm 的色谱柱可提供多达 45,000 个芳香烃理论塔板，或约 5.5 μm 的最小塔板高度，最佳线速度约为 15,000 微米。乙腈-水（80/20，v/v）流动相，40℃，压力2.3 mm/s，背压7.5 MPa。该柱的渗透率与填充5 μ m颗粒的色谱柱相似，K-F约为2.4×10(-14) m(2)（基于流动相的空塔线速度），而塔板高度值与填充5 μ m颗粒的色谱柱相当。 2.5μm颗粒。通过采用两个或三个串联的 25 cm 色谱柱，可以在背压低于 30 MPa 的情况下生成 80,000-120,000 块理论塔板。与传统的整体式硅胶柱或颗粒柱相比，长柱的使用能够容易地产生大量的理论塔板。动力学图分析表明，在理论塔板数 (N) 大于 50,000 的范围内，在 30 MPa 下运行的整体柱可以比在 40 MPa 下运行的全多孔 3-μm 颗粒填充的柱提供更快的分离。 (C) 2010 Elsevier B.V. 保留所有权利。
Chromatographic properties of a new type of monolithic silica rod columns were examined. Silica rod columns employed for the study were prepared from tetramethoxysilane, modified with octadecylsilyl moieties, and encased in a stainless-steel protective column with two polymer layers between the silica and the stainless-steel tubing. A 25 cm column provided up to 45,000 theoretical plates for aromatic hydrocarbons, or a minimum plate height of about 5.5 mu m, at optimum linear velocity of ca. 2.3 mm/s and back pressure of 7.5 MPa in an acetonitrile-water (80/20, v/v) mobile phase at 40 degrees C. The permeability of the column was similar to that of a column packed with 5 mu m particles, with K-F about 2.4 x 10(-14) m(2) (based on the superficial linear velocity of the mobile phase), while the plate height value equivalent to that of a column packed with 2.5 mu m particles. Generation of 80,000-120,000 theoretical plates was feasible with back pressure below 30 MPa by employing two or three 25 cm columns connected in series. The use of the long columns enabled facile generation of large numbers of theoretical plates in comparison with conventional monolithic silica columns or particulate columns. Kinetic plot analysis indicates that the monolithic columns operated at 30 MPa can provide faster separations than a column packed with totally porous 3-mu m particles operated at 40 MPa in a range where the number of theoretical plates (N) is greater than 50,000. (C) 2010 Elsevier B.V. All rights reserved.