Font Size: a A A

Preparation Of Poly(TAIC-co-TMPTA)Monolith And Investigation Of Its Chromatographic Characteristics

Posted on:2015-03-04Degree:MasterType:Thesis
Country:ChinaCandidate:J ZhongFull Text:PDF
GTID:2251330422469955Subject:Drug Analysis
Abstract/Summary:PDF Full Text Request
High performance liquid chromatography (HPLC) technique is undoubtedly one of thecornerstones of modern analytical chemistry. Monolithic columns have been developedrapidly for their advantages of low back pressure drop, fast mass-transfer, simple preparationand versatile modes to be modified and therefore monolithic columns have been widely usedin liquid chromatography (LC).Firstly,a new polymeric monolithic column was prepared by in situ polymerization. Inthe polymerization, triallyl isocyanurate (TAIC) was used as the functional monomer,trimethylolpropane triacrylate (TMPTA) as the crosslinking agent, polyethylene glycol200and1,2-propanediol as the co-porogens,2,2-azobisisobutyronitrile as the initiator. Theresultant best monoliths were optimized by adjusting the ratio of TMPTA to TAIC and thecomposition of porogenic solvent. The resulting monolith showed a relatively homogeneousstructure, good permeability and mechanical stability. These applications demonstrated thatthe monoliths could be successfully used as the HPLC stationary phase to separate smallmolecules from the mixture. At the optimized flow rate of1.0mL min-1, theoretical platenumber was more than8,000plates m-1.Secondly, poly(TAIC-co-TMPTA) monolithic column was synthesized by atom transferradical polymerization technique. Morphology of the prepared polymeric monolith wasinvestigated by the scanning electron microscopy; pore properties were assayed by mercuryporosimetry and nitrogen adsorption. The column was used as the stationary phase of reversedphase high performance liquid chromatography (RP-HPLC) and capillary liquidchromatography (CLC) to separate the mixture of aromatic compounds. In the CLC system,four analytes were separated with the flow rate of2.0μL min1in9min. The new columnperformed around125,000theoretical plates per meter. The column showed goodreproducibility: the relative standard deviation values of the retention factor values foraromatic compounds were less than1.52%(n=7).
Keywords/Search Tags:Organic monolithic column, High Performance Liquid Chromatography (HPLC), Capillary liquid chromatography (CLC), Atom transfer radical polymerization (ATRP), Small molecules
PDF Full Text Request
Related items