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手性金属-有机骨架材料(MOFs)作为一种新型多孔材料,由于具有比表面积大、结构多样、孔尺寸可调和化学稳定性良好等特点,而备受色谱分离领域的关注。该文以(1R,2R)-1,2-环己烷二甲酸(H_2L)和4,4′-联吡啶(bpy)为配体与铜离子反应,通过溶剂热法合成了一种具有二维手性网状结构的手性MOF[Cu_3(HL)_2(L)_2(bpy)_3]·4H_2O。将该手性MOF作为手性固定相制备了高效液相色谱柱。为了考察MOF[Cu_3(HL)_2(L)_2(bpy)_3]·4H_2O的手性识别能力,在正相色谱(流动相:正己烷-异丙醇)条件下,对一系列外消旋化合物在手性MOF柱上进行了拆分。该手性MOF柱对醇类、酮类、酸类、环氧化合物和醚类等10种手性化合物表现出较好的拆分效果。对该手性MOF柱的重现性、稳定性作了评价,考察了进样量对分离效果的影响,结果表明该手性MOF柱具有较好的重现性和稳定性。
As a new type of porous materials, chiral metal-organic framework materials (MOFs) have attracted much attention in the field of chromatographic separation because of their large specific surface area, diverse structures, adjustable pore size and good chemical stability. In this paper, (1R, 2R) -1,2-cyclohexanedicarboxylic acid (H_2L) and 4,4’-bipyridine (bpy) were used as ligands to react with copper ions. The chiral MOF [Cu_3 (HL) _2 (L) _2 (bpy) _3] · 4H_2O of the chiral reticular structure. High performance liquid chromatography (HPLC) columns were prepared using the chiral MOF as a chiral stationary phase. In order to investigate the chiral recognition ability of MOF [Cu_3 (HL) _2 (L) _2 (bpy) _3] · 4H_2O, a series of racemic reactions were carried out in normal phase chromatography (mobile phase: n-hexane-isopropanol) The compound was resolved on a chiral MOF column. The chiral MOF column showed good resolution for 10 chiral compounds such as alcohols, ketones, acids, epoxides and ethers. The reproducibility and stability of the chiral MOF column were evaluated. The effect of injection volume on the separation efficiency was investigated. The results showed that the chiral MOF column has good reproducibility and stability.