Multi-modes Silica-based Chromatographic Materials:Preparation And Their Separation Performances

With the increasing demands for the separation and analysis of complex samples,it is of great significance to develop new chromatographic stationary phases with multi-modes.In this work,ionic liquid and surfactant with good solubility for proteins and other biomolecules were selected as functionalized reagents to fabricate new stationary phase.The separation and analysis performances of the developed columns were initially evaluated.The full text divided into five chapters.In the first chapter,five parts are included.The first part briefly describes the high performance liquid chromatography stationary phases.The second part briefly describes the applications of ionic liquids in separation and analysis.The third part briefly describes the applications of surfactants in separation and analysis.The fourth part briefly introduces the research idea of this thesis.In the second chapter,with sodium undecylenate（NaUA）as the functionalized monomer,it was facilely grafted onto the surface of thiol-functionalized silica gels via a one-step click reaction.The structure of the Sil-NaUA stationary phase was characterized by Fourier transform infrared spectrometer and thermogravimetric analysis,respectively.The results demonstrate that the Sil-NaUA stationary phase was successfully prepared.Furthermore,the packed Sil-NaUA column indicates typical hydrophilic interaction liquid chromatography retention characteristic.It can be used for separation of hydrophilic nucleosides and nucleic acid bases,amides,flavonoids and sulfonamides with good separation efficiency.In the third chapter,with 1-vinyl-3-dodecyl imidazole bromide（VDI）as the functionalized monomer,it was also grafted onto the surface of thiol-functionalized silica gels via the one-step click reaction.The Sil-NaUA stationary phase was characterized by Fourier transform infrared spectrometer and thermogravimetric analysis,respectively.The results demonstrate that the Sil-NaUA stationary phase was successfully prepared.The packed Sil-VDI column possesses typical reversed-phase liquid chromatography and ion-exchange chromatography mixed-mode retention mechanisms.Thus,alkylbenzenes,polycyclic aromatic hydrocarbons,anilines,phenols,benzene derivatives as well as inorganic anions BrO₃^-,NO₃^-and IO₃^-were selected to test the separation performances of the column.Moreover,the Sil-VDI column also shows certain separation potential for protein samples.In the fourth chapter,the Sil-NaUA and Sil-VDI columns were further applied for the separation and analysis of phospholipid extracts from lung adenocarcinoma cells and egg yolk and the separation performances of the two columns were further compared.Compared with Sil-NaUA column,the mixed-mode Sil-VDI column shows better separation and analysis selectivity.In our future research,we will explore the potential of the developed stationary phases for separation of versatile biological samples.In the fifth chapter,the full work was summarized.