电渗泵毫米整体柱电色谱联用测定食品防腐剂分析化学专业论文.docxVIP

ABSTRACTABSTRACT ABSTRACT ABSTRACT Electrokinetic flow analysis(EFA)system is based on sequential injection analysis (StA)， multicommutation analysis， electroosmotic delivery and chromatographic separation．The EFA system possesses its advantages of simplicity, convenience，multifunction and controllability．The main aim of this thesis is to extend its analytical function and application．A 2．0 mnl i．d．Cs-silica monolithic column was prepared by one·step polymerization．The preparation conditions of the reversed-phase silica monolithic microcolumn filled with fine quartz sand and its chromatographic separation behavior were studied．In addition，the prepared microcolumn has been employed in the separation of parabens by reversed-phase chromatography and electrochromatography (EC)delivered by pressure／electroosmosis flow successflly． 1．Silica monolithic chromatography columns functionalized with octyl groups were synthesized by one—step polymerization from tetrathoxyailane(TEOS)and n·-octyltriethoxsiliane(Cs·-TEOS)hydrolyzed by acid and polymerized under base conditions．The influence factors in the sol-gel procedure were investigated，such as acidic concentration and reaction time．The optimal preparation conditions are listed as follows：0．5 mL TEOS，0．4 mL Cs-TEOS，0．6 mL ethanol，0．10 mL 0．016 mol／L HCl were mixed for 1 min，hydrolyzed at 600C for 6 h and cooled to room temperature．N—dodecylamine of 25 mg was added into the sol-gel solution，and then the mixed solution was introduced into a PTFE mold,and polymerized at 600C for 45 h．The micromorphology and element analysis results of the monolithic column validated that the microcolumn could be employed in the chromatographic separation． For the preparation of the silica monolithic column mentioned above，the microcolumns were prepared in a 2．0 toni i．d．fused-silica tube filled with 1 00-1 20 lxm quartz sand to avoid column shrinkage．Three parabens were separated on baseline using the silica monolithic microco