Optimization of binary porogen solvent composition for preparation of butyl methacrylate monoliths in capillary liquid chromatography.
Butyl methacrylate monolithic columns in 320 microm i.d. fused silica capillaries for reversed-phase capillary liquid chromatography were prepared by radical polymerization initiated thermally with azobisisobutyronitrile (AIBN). Polymerization mixture contained butyl methacrylate (BMA) as the function monomer and ethylene dimethacrylate (EDMA) as the crosslinking agent with 1,4-butanediol and 1-propanol as a binary porogen solvent. Ratio of 1,4-butanediol to 1-propanol in the porogen solvent was optimized regarding the monolithic column efficiency and performance. Total porosity, column permeability, separation impedance, Walters hydrophobicity index, retention factors, peak asymmetry factors, height equivalents to a theoretical plate and peak resolutions were used for characterization of the prepared monolithic columns. The polymerization mixture consisting of 17.8% of BMA, 21.8% of EDMA, 18.0% of 1,4-butanediol, 42.0% of 1-propanol and 0.4% AIBN generated monolithic columns of the best performance having a sufficient permeability and the lowest separation impedance. It was also demonstrated that monolithic columns of this composition exhibited good preparation reproducibility and an excellent pressure resistance when applied in capillary liquid chromatography.
Grafnetter
Jan
J
Department of Analytical Chemistry, Faculty of Science, Charles University, Albertov 2030, 12840 Prague, Czech Republic.
Coufal
Pavel
P
Tesarová
Eva
E
Suchánková
Jana
J
Bosáková
Zuzana
Z
Sevcík
Juraj
J
D019075:Electrophoresis, Capillary; D008689:Methacrylates / Q000737:chemistry*; D011108:Polymers / Q000138:chemical synthesis; D015203:Reproducibility of Results; D012997:Solvents; D013056:Spectrophotometry, Ultraviolet
D008689:Methacrylates; D011108:Polymers; D012997:Solvents; C016284:butyl methacrylate