Font Size: a A A

TITLE Preparation Of Novel Chiral Statinonary Phases And Their Applications In Capillary Electrochromatography

Posted on:2010-10-17Degree:DoctorType:Dissertation
Country:ChinaCandidate:X L DongFull Text:PDF
GTID:1101330332983158Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
Capillary electrochromatography (CEC) has becoming one of the most promising analytical technique in chiral separation science. The preparation of capillary chiral stationary phases (CSPs) are the focus of this technique. The objective of this thesis is to develop new methods to prepare novel CSPs for separation of enantiomers by CEC.Vancomycin was first immobilized onto the silica-based monolithic capillary columns. After the optimization of the immobilization and separation conditions, six pairs ofβ-blockers were resolved under polar organic mode and another two pairs of ennatiomers were resolved under reversed phase mode by CEC. Very high column efficiency was achieved for the resolutions. The prepared chiral columns could be used for fast-speed enantioseparations.Cellulose tris(3,5-dimethylphenylcarbamate) was successfully bonded onto the surface of silica monolith by regio-selective approach. When this prepared CSP was used to separate enantiomers in CEC, six pairs of enantiomers were resolved. The adoption of THF as mobile phase modifier improved the separation of praziquantel.Cellulose tris(3,5-dimethylphenylcarbamate) was coated onto positively charged polyacrylamides monolith. Compared with the monolithic silica gel, the organic monolith embraced better pH stability and more substantial EOF. These superior properties extended the application areas of enantiomers and widened the applicable pH ranges of the mobile phases. Tweleve pairs of ennatiomers, including acidic, basic and neutral compounds, were resolved successfully.Mesoporous silica nanoparticles (MCM-41) immobilized open-tubular capillary column with coating of cellulose tris(3,5-dimethylphenyl-carbamate) was prepared. The surface area of the fused silica capillary column was greatly improved by immobilizing homemade MCM-41 nanoparticles onto the inner-wall; and consequently, improved the coating amount of cellulose derivatives. Eight pairs of ennatiomers were successfully resolved. Compared with the particulated and monolithic CSPs, the native CSP showed the advantages of easy preparation and convenient operation.Lysine bonded zwitterionic Poly (GMA-co-EDMA) monolithic capillary column was prepared for CEC separation. Aromatic compounds, phenols, acids, anilines and basic drugs were successfully separated on the zwitterionic monolithic capillary column as the strength and direction of EOF can be easily adjusted by varying the pH values of running buffers through changing the ionization of those groups on lysine molecule. The prepared organic monolith showed the potential application in chiral separation.
Keywords/Search Tags:Chiral stationary phases, Monolithic column, Open-tubular column, Enantioseparation, Capillary elctrochromatography
PDF Full Text Request
Related items