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将10°锥角台锥型液相色谱柱放大至150mm长、入口直径54mm、出口直径27mm,容积为200mL,填料为粒径40～75μm、孔径11nm的C18球形硅胶。流动相在锥型柱内呈现塞子状流形。系统地评价了该柱的分离性能,结果表明:在最佳流速为6mL/min时,以萘峰计,锥型柱的折合理论塔板高度为2.11,柱效下降10%时的样品质量和体积载样量分别为2.1mg和1.7mL,与同长度同体积圆柱型柱相比,柱效提高了20%,质量载样量提高了16%以上,体积载样量提高了19%以上。当进样质量由2.4mg增加到12mg时,对羟基苯甲酸乙酯峰与对羟基苯甲酸丁酯峰的分离度(Rs2)由2.14降到1.71,对羟基苯甲酸丁酯峰与萘峰的分离度(Rs3)由2.91降到2.52;当进样体积由3mL增加到19mL,Rs2由2.23降到1.28,Rs3由2.95降到2.30,但此时的色谱峰峰形仍然高度对称,没有拖尾,有利于从基质中制备分离微量组分。实验结果表明锥型液相色谱柱将具有广泛的应用前景。
The 10 ° cone conical liquid chromatography column was enlarged to 150 mm in length with an inlet diameter of 54 mm, an outlet diameter of 27 mm and a volume of 200 mL. The filler was C18 spherical silica with a particle size of 40 to 75 μm and a pore size of 11 nm. The mobile phase presents a plug-like manifold within the conical column. The separation performance of the column was systematically evaluated. The results show that the theoretical plate height of cone column is 2.11 when the optimum flow rate is 6mL / min, and the sample mass and The volumetric loadings were 2.1mg and 1.7mL respectively. Compared with the same length cylindrical column, the column efficiency increased by 20%, the mass loading amount increased more than 16% and the volume loading volume increased more than 19%. When the injection mass increased from 2.4mg to 12mg, the separation of ethylparaben and butylparaben peak (Rs2) decreased from 2.14 to 1.71. The butylparaben peak and naphthalene peak The resolution (Rs3) decreased from 2.91 to 2.52. When the injection volume increased from 3 mL to 19 mL, the Rs2 decreased from 2.23 to 1.28 and the Rs3 decreased from 2.95 to 2.30. However, the chromatographic peak shape at this time was still highly symmetrical with no tailing , Which facilitates the preparation of the separation of trace components from the matrix. Experimental results show that conical liquid chromatography columns will have a wide range of applications.