葫芦[6]脲单轮烷键合固定相的制备、表征及色谱性能

Preparation, Characterization and Chromatographic Performance of Cucurbit[6]uril Monorotaxane Bonded Silica Stationary Phase

将超分子自组装技术与色谱键合硅胶固定相制备技术相结合,采用γ-[(2,3)-环氧丙氧]丙基三甲氧基硅烷(KH-560)为偶联剂,首次将一种葫芦[6]脲单轮烷(CB6MR)键合到硅胶上,制备了一种新型的葫芦[6]脲单轮烷键合固定相(CB6MRBS).通过元素分析、红外光谱和热分析对该固定相进行了结构表征.以中性、酸性、碱性化合物和二取代苯位置异构体等溶质为样品,分别在反相和正相色谱模式下对固定相的色谱性能和保留机理进行了研究.结果表明:CB6MRBS是一种多模式键合固定相,具有良好的正相和反相色谱性能,对位置异构体具有较高的识别能力,尤其是可有效地用于碱性化合物的分离分析.其保留机理存在氢键、静电、π-π和疏水作用等多种作用力机制,协同作用提高了CB6MRBS对溶质的分离选择性.由于CB6MR配体中含有酰胺基和众多羰基,CB6MRBS可能在络合色谱方面有应用前景.

A novel cucurbit[6]uril monorotaxane formance liquid chromatography has been bonded silica stationary phase （CB6MRBS） for high perprepared successfully by combining supramolecular self-assembly technology with the immobilization technique of chromatography stationary phase. A cucurbit[6]uril monorotaxane （CB6MR） was, for the first time., grafted to silica gel by using γ-glycidoxypropyltrimethoxysilane （KH-560） as a coupling reagent. CB6MRBS was characterized by FTIR, elemental analysis and thermal analysis. The chromatographic performance and retention mechanism of the new packing material were evaluated by using organic components including acidic, basic, neutral analytes and positional isomers of disubstituted benzene as probe molecules under reversed-HPLC and normal-HPLC mobile phases. The results show that CB6MRBS is a sort of multimode bonded stationary phase with excellent reversed-phase and normal-phase chromatographic properties. CB6MRBS shows obvious priority for separation of positional isomers, especially for the efficient separation of basic compounds. The new packing material can provide various action sites for different analytes, such as those of hydrogen-bonding, π-π, electrostatic and hydrophobic interactions. It may have good prospect for complexation chromatography, which is required to further study.