Synthesis And Chromatographic Evaluation Of Several Cellulose Chiral Stationary Phases And Polymer Matrix Hydrophilic Stationary Phases

High performance liquid chromatography?HPLC?is one of the most widely used separation methods,owing to its advantages of high separation efficiency and fast analysis speed.The core of HPLC lies on the chromatographic column,in which the packing materials determined the separation performance.Therefore,developing new HPLC packing materials has attracted a lot of chromatographers'attention,to enrich the categories for varied separation purposes.In addition,as the continuous development of pharmaceutical industry and food industry,the separation of chiral compounds and strongly polar compounds is highly desired.As a result,it is particularly important to prepare new stationary phases for the separation of chiral or strongly polar substances.Based on the above analysis,this thesis focuses on the“development of new stationary phases for these two aims”:1.Cellulose tris 4-methylphenylcarbamate?CTMPC?was synthesized using"non-regional selection"method.CSP1,CSP2 and CSP3 were prepared by coating CTMPC on SiO₂ 1?²?m,flow-through silica?,SiO₂ 2?⁵?m,flow-through silica?and SiO₂ 3?⁵?m,commercial silica?accordingly.The separation performance,column pressure and application of the three kinds of CSPs in rapid chiral separation were compared.CSP1 showed the strongest selectivity and the shortest retention time with the similar loading amount for the five chiral analytes investigated,i.e.tr?ger's bases,tebuconazole,hexaconazole,econazole nitrate and diniconazole.What's more,the column efficiency was less dependence of the flow rate,which showed the great potential of SiO₂ 1 in the filed of fast chiral separation.In addition,flow-through silica possessed lower pressure than commercial silica with the same size due to its pore structure characteristics,which provided high pressure resistance for the application of fast chiral separation.The influence of column temperature on the retention of the five chiral substances on three kinds of CSPs was investigated The retention of five chiral compounds on CSP1,CSP2and CSP3 was an exothermic process based on enthalpy control,and low temperature was conducive to the separation of these chiral compounds.2.Mesoporous melamine-formaldehyde resin microspheres?MMFRS?were prepared by suspension polymerization and used as the HPLC stationary phase.The retention mechanism of MMFRS was explored by changing a series of factors comprising the proportion of ACN,buffer salt concentration,pH and column temperature.The results showed that MMFRS exhibited the property of HILIC mode in the region with high acetonitrile content,and the reversed phase in the region with low acetonitrile content,which demonstrated that the MMFRS provided the combined mechanism of hydrophilic interaction chromatography and reversed phase chromatography.In addition,the exploration in the separation of artificial sweeteners demonstrated the great potential of MMFRS in the analysis of hydrophilic compounds.3.The homemade polystyrene-divinyl benzene?PS-DVB?was coated by the crosslinked polyethleneimine?PEI?,giving PS-DVB-PEI-GA stationary phase.The stationary phase could provide ion exchange,hydrogen bonding and electrostatic interaction for the retention of analytes.In addition,the PS-DVB-PEI-GA displayed good stability and revealed good separation performance on water-soluble vitamin samples in the HILIC mode.4.The synthesis,characterization and application of eight kinds of chiral separation materials were reviewed in order to provide references for researchers to develop new chiral separation selectors.