Study On Preparation And Property Of Marocycle Supramolacular Bonded Stationary Phases For High Performance Liquid Chromatography

Macrocycle supramolecular bonded silica stationary phases have been gaining great interest for the chromatography due to especial molecular recognition based on supramolecular interaction retention mechanism. It is necessary to explore new preparation process of the stable bonded silica stationary phases with macrocycle molecules. In addition, cyclodextrin and calixarene as host molecules of the second and third generation supramolecular to possess molecular recognition ability is an attractive research object in overlapping area of modern separation science with biomedical and material sciences, showing great promising prospect to develop the supramolecular theory and application in chromatography. In the dissertation, the preparation method and characterization of novel p-cyclodextrin andp0terf-calix[8]arene bonded silica stationary phases for high performance liquid chromatography were studied, their chromatographic performance were evaluated systematically and retention mechanisms were researched. The major contents are as follows:l.The preparation, evaluation, application and retention mechanism of p-cyclodextrin and calixarene bonded silica stationary phases for high performance liquid chromatography were reviewed in detail, which provides the basis for further research of other new bonded stationary phases and which is the foundation for new ideas, object and design of technical scheme of the dissertation.2 A newp-tert-calix[8]arene bonded silica stationary phase (CBS) for high performance liquid chromatography was prepared firstly by condensation reaction on solid surface of silica between the sodium of p-terr-calix[8]arene and bonded chloropropyl groups which were obtained by reaction of chloropropyltriethoxysilane with silica. The stationary phase was characterized by elemental analysis, FTIR and thermoanalysis. The chromatographic performance of CBS was studied by using PAHs, allkylbenzene and disubstituted benzenes as solutes and compared with mat of CPS and ODS; and the retention mechanism, column efficiency and peak symmetry were also studied. The result shows that the stationary phase has reversed-phase chromatographic performance and especial separation selectivity. Good selectivity, symmetry peak and high column efficiency were obtained for disubstituted benzenes particularly aniline compounds, which make up the disadvantage of ODS. Chromatographic process exist various retention mechanism based on the supramolecular interaction, such as hydrogen-bonding, p-p charge-transfer, dipole-dipole interaction andinclusion complexation and hydrophobic interaction.3.The high performance liquid chrornatographic behavior of some steroid hormone medicines was studied on CBS. The effect of mobile phase variable such as methanol content, pH values, ionic strength and cation type of buffer was investigated. It is found that the solutes were separated respectively on CBS, CPS and ODS, but the elution order and separation selectivity were difference among three stationary phases, which means the different retention mechanism exist among three stationary phases. For multi-retention mechanisms exhibit on CBS, the separation selectivity was improved for solutes with the similar hydrophobicity whennd hydrogen-bonding interaction exist between solutes and stationary phase. In addition, the separation speed was increased due to weaker hydrophobicity of CBS compared with ODS, gradient elution was avoided and consumption of organic solvent was decreased for me separation of the solutes with very different hydrophobicity.4. A novel P -cyclodextrin bonded silica stationary phase ( 3 CD-BS) for high performance liquid chromatography was prepared firstly by condensation reaction on solid surface of the bonded silica between the sodium of cyclodextrin and bonded chloropropyl groups. The stationary phase was characterized by elemental analysis and FTIR. The chromatographic performance and retention mechanism of 3 -CD-BS were studied by using PAHs, allcylbenzene, disubstituted benzenes, substituted benzene, phenol c...