| With various chromatographic stationary phases appearing, It has effectively promoted the chromatographic theory and separation technology to improve and develop, and solved a variety of complex problems in the areas of separation and analysis, research in stationary phase of chromatography has become is an important task. Since Delville and his coworkers reported the application of ferrocene as the stationary phase, it has attracted extensive attention in liquid chromatography due to its varieties of separation mechanisms, including hydrophobic, hydrogen bonding,π-π, dipole-dipole and charge-transfer interactions. In recent years, this type of ferrocene organic metal bonded stationary phase in practice highlights the advantages, it possess normal and reversed phase chromatography performance, and it can meet the actual sample testing requirements. Therefore we based on existing research, combined with the advantages of nitrogen containing compound based stationary phase, the use of nitrogen-containing groups to strengthen the force between the stationary phase and the analyte, its spatial effect can be well masked silica surface silanols activity, improve chromatographic peak, the advantage of improved sensitivity analysis. Therefore, we will develope new ferrocene-bonded stationary phase and expand the application of ferrocene ligand based on our research basis.In this paper, two new silica-bonded stationary phases and a solid phase extraction packing with ferrocene as skeleton material were synthesized. Also, its chromatographic behaviors were studied. The main contents are as following:1 、 4-chloro-6-pyrimidinyl ferrocene-bonded silica stationary phase was synthesized, and characterized by infrared spectroscopy, elemental analysis and thermogravimetricanalysis. Linear solvation energy relationship method was successfully employed to evaluate the new phase. The results showed that it has positive and reverse-phase chromatography performance. With chromatographic performance experiments to explore, the stationary phase exhibits good separation effect, can effectively mask of residual silanols. Different series of analytes includingPAHs, mono-substituted benzenes, aromatic amines, phenols, quinolines, pyridines,nucleosides and inorganic anions were successfully separated on this novel multi-interaction stationary phase, respectively. It also seems hydrophobic and hydrophilic properties. The multi-interaction mechanism including hydrophobic, π-π,hydrogen-bonding, charge-transfer, acid-base equilibrium and anion-exchange interactions is involved in the chromatographic separation; Furthermore, the NFcS column was successfully employed for the analysis of plant growth regulators in fruits and vegetables.2 、 4-chloro-6-pyrimidinyl ferrocene solid phase extraction packing was synthesized, The NFc Si enables a more efficient purification and enrichment of sulfonamide from a complex matrix due to its multi-interaction ability. We discussed the different conditions for solid phase extraction efficiency, and optimized pre-treatment methods, a HPLC method based on the new NFcSi-SPE cleanup has been successfully employed for the purification and determination of sulfonamide in pork, egg, milk, and honey samples with complex matrices.3、N-ferrocenyl benzoyl-(1S, 2R)-1,2- diphenyl ethanol bonded silica stationary phase was synthesized, The structure of new material was characterized by infrared spectroscopy, elemental analysis and thermogravimetricanalysis and so on.polycyclic aromatic hydrocarbons, amines, phenols, nitroimidazoles, quinoline,nucleosides, nitroaniline positional isomers were successfully separated under reversed phase conditions; racemate of DL- phenylalanine and DL- valine were split under normal phase conditions. The results show that the stationary phases of different solutes multiple forces, including hydrophobic, hydrogen-bonding, π-π,charge-transfer, dipole-dipole interaction. It can offer the possibility for a variety of solutes of separation. |
PDF Full Text Request