Preparation Of Hydrophilic Monolithic Column And Its Application In Pressurized Capillary Electrochromatography

Monolithic column for capillary electrochromatography was developed along with the development of the chromatography separation technology as a new type of separation methods,because of its mass transfer speed,anti depress,high column efficiency,known as the fourth generation of separation medium.Hydrophilic effect chromatography(hydrophilic interaction liquid chromatography,HILIC)due to the separation of polar compounds,when connected with mass spectrometry,chromatographic without hydrophilic effect ion of reagent,convenient and economy,in recent years has been the great concern of people.In this thesis,three kinds of hydrophilic monolithic columns which are poly(SPP-co-PETA-Me OH&PEG),poly(AMPS-co-PETA-Et OH&PEG)and poly(POSS-co-AM-THF)were prepared.They are applied in the pressurized capillary electrochromatography(p CEC)system to study their separation theory.And the separation of the mixtures are quite good.The thesis contains seven chapters as follows:The first chapter introduced the basic theory of capillary electrochromatography and pressurized capillary electrochromatography.Further,it reviewed the theoretical research and the overall progress of the monolithic column,which provided a theoretical basis and methods for the project.The second chapter described the preparation,optimization and characteration of the organic polymer monolith column poly(SPP-co-PETA-Me OH&PEG)in detail.Sulfobetaine-based capillary zwitterionic hydrophilic monolithic column was synthesized with a novel binary porogenic agent of polyethylene glycol(PEG)/methanol.The polymer was prepared with SPP as monomer,PETA as crosslinker,AIBN as initiator.In order to optimize the properties,the contents of the polymerization mixture were investigated.The optimum preparation conditions were as followed: monomer: porogenator(1:2);monomer(SPP:PETA=1:1);the binary porogenic agent(PEG:methanol=1:1.5);composition of the initiator(AIBN)was 0.1%.With the binary porogenic agent of PEG/methanol addition,good mechanical stability,homogeneous column bed,good permeability and narrow pore size distribution were obtained.In the third chapter,the columns poly(SPP-co-PETA-Me OH&PEG)was used in capillary liquid chromatography(c LC)for the separation of a mixture of phenols,amines and benzene compounds.The fourth chapter described the preparation,optimization and characteration of the organic polymer monolith column poly(AMPS-co-PETA-Et OH&PEG)in detail.It was prepared with AMPS,PETA,in porogenic agents consist of Et OH and polyethyleneglycol-6000,with the help of initiator AIBN.In order to optimize the properties,the contents of the polymerization mixture were investigated.The optimum preparation conditions were as followed: monomer: porogenator(1:3);monomer(AMPS:PETA=1:1);the binary porogenic agent(PEG:Et OH=1:3);composition of the initiator(AIBN)was 0.1%.With the binary porogenic agent of PEG/ Et OH addition,good mechanical stability,homogeneous column bed,good permeability and narrow pore size distribution were obtained.In the fifth chapter,the poly(AMPS-co-PETA-Et OH&PEG)columns were used in pressurized capillary electrochromatography(p CEC)for the separation of a mixture of phenols,amines,nucleosides and heterocyclic compounds.The sixth chapter described the preparation,optimization and characteration of the organic polymer monolith column poly(POSS-co-AM-THF)in detail.It was prepared with POSS and AM in porogenic agents consist of THF,with the help of initiator AIBN.In order to optimize the properties,the contents of the polymerization mixture were investigated.The optimum preparation conditions were as followed: monomer: porogenator(1:5);monomer(POSS:AM=1:5);composition of the initiator(AIBN)was 0.1%.In the seventh chapter,the poly(POSS-co-AM-THF)columns were used in p CEC for the separation of a mixture of amines,nucleosides,nitrobenzene nmines and benzene compounds.