C18反相色谱固定相的制备及性能评价
Preparation and Performance Evaluation of C18 Stationary Phase for Reversed-Phase Chromatography
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摘要: 以粒径10 μm硅胶为基质,与1,6-六亚甲基二异氰酸酯和十二醇反应制得新型C18反相色谱固定相。热失重结果表明,所制得的固定相在200 ℃以内热稳定性良好。扫描电镜结果表明:硅胶在改性前后没有损坏,颗粒完整,适合于色谱柱的填装。该固定相对联苯的静态吸附在4 h时达到平衡,吸附行为符合Langmuir吸附等温式。用芳香烃和极性化合物对固定相的分离性能进行评价,结果表明所合成的固定相具有良好的色谱性能。Abstract: Novel C18 stationary phase for reversed-phase chromatography was prepared through the reaction of 1,6-diisocyanatocyclohexane and dodecanol with silica gel ( 10 μm) as matrix. It was shown by the result of thermogravimetry, the stationary phase behaved to have good thermal stability below 200 ℃. As shown by the result of SEM, the silica gel was kept undamaged before and after denaturing and was suitable for packing into the chromatographic column. It was found that the static adsorption of biphenyl on the stationary phase attained to equilibrium after 4 h. The adsorption behavior of the stationary phase was found to conform with the Langmuir isotherm. The separation capability of the stationary phase was evaluated by using aromatic and polar compounds as sample. It was shown that the stationary phase displayed good chromatographic properties.