Lu Liejuan, Chen Jie, Guan Yafeng
Department of Instrumentation & Analytical Chemistry, Dalian Institute of Chemical Physics, the Chinese Academy of Sciences, Dalian 116023, China.
Se Pu. 2009 May;27(3):299-302.
A preparative scale liquid chromatographic column with the conical shape of 10 degrees opening angle was constructed and evaluated. The column was designed with the inlet/outlet diameters of 54/27 mm, the column length of 150 mm and the column volume of 200 mL, and packed with the spherical C18 bonded silica with the particle size of 40-75 microm and the aperture of 11 nm. The mobile phase in the conical column showed a plug like flow profile and plug like chromatographic band shape. For naphthalene, the reduced plate height was about 2.11; the maximum sample load was 2.1 mg or 1.7 mL (10% reduction of plate number), which is 20%, 16% and 19% higher than that of cylindrical one of the same length and volume. As the injection mass increased from 2. 4 mg up to 12 mg, the resolution of ethyl paraben/butyl (R, ) reduced from 2. 14 down to 1.71, and the butyl paraben/naphthalene (Rs3) from 2.91 down to 2.52; the injection volume increased from 3 mL up to 19 mL, Rs2, reduced from 2.23 down to 1.28, and Rs3 from 2.95 down to 2.30, while the peaks were still in symmetric shape without tailing. This characteristic of the column shall benefit for the separation of trace components from matrix. This demonstrated the conical shaped preparative columns would have a broad practical applicability for obtaining pure compounds.
构建并评估了一种开口角度为10度的锥形制备规模液相色谱柱。该柱的进样口/出口直径设计为54/27毫米，柱长150毫米，柱体积200毫升，并填充了粒径为40 - 75微米、孔径为11纳米的球形C18键合硅胶。锥形柱中的流动相呈现出类似塞子的流动轮廓和类似塞子的色谱带形状。对于萘，折合塔板高度约为2.11；最大进样量为2.1毫克或1.7毫升（塔板数降低10%），比相同长度和体积的圆柱形柱高20%、16%和19%。随着进样质量从2.4毫克增加到12毫克，对羟基苯甲酸乙酯/丁酯的分离度（Rs2）从2.14降至1.71，对羟基苯甲酸丁酯/萘的分离度（Rs3）从2.91降至2.52；进样体积从3毫升增加到19毫升时，Rs2从2.23降至1.28，Rs3从2.95降至2.30，而峰仍呈对称形状且无拖尾。该柱的这一特性有利于从基质中分离痕量组分。这表明锥形制备柱在获得纯化合物方面具有广泛的实际应用价值。
