Abstract
Organic monolithic columns with high efficiency were obtained for use in capillary electrochromatography (CEC) from a mixture of monomers (constant concentrations) with different proportions of porogenic solvents (1,4-butanediol with isoamyl alcohol, amyl alcohol or cyclohexanol in the presence or absence of water). The stationary phases were prepared from the precursor monomer octadecyl methacrylate (ODMA), the cross-linking agent ethylene dimethacrylate (EDMA) and the ionizable monomer 2-acryloylamido-2-methylpropanesulfonic acid (AMPS), the latter being necessary to make the stationary phase negatively charged, assuring electrosmotic flow (EOF) during analysis. The monolithic columns synthesized were physically characterized by porosimetry and scanning electron microscopy (SEM), and electrochromatographically characterized by calculation of chromatographic parameters. The most efficient column was prepared using the porogenic solvent amyl alcohol:1,4-butanediol in a 65:35 (v/v) ratio and showed a plate height of 38 µm. These columns were applied for the separation of alkyl parabens and polycyclic aromatic hydrocarbons (PAH).
Highlights
Capillary electrochromatography (CEC) is a hybrid technique of capillary electrophoresis (CE) and high performance liquid chromatography (HPLC).[1,2] The capillary electrochromatography (CEC) technique can be defined as a type of capillary electrophoresis carried out in packed capillary columns in an environment in which an applied electric field is responsible for the movement of the mobile phase across the capillary, generating the electrosmotic flow (EOF).[3]
The CEC technique can be defined as a type of capillary electrophoresis carried out in packed capillary columns in an environment in which an applied electric field is responsible for the movement of the mobile phase across the capillary, generating the electrosmotic flow
The high efficiency obtained with the use of the CEC technique is due to the EOF profile, that is different of the profile achieved by the pressure application, occurred at the HPLC technique
Summary
Capillary electrochromatography (CEC) is a hybrid technique of capillary electrophoresis (CE) and high performance liquid chromatography (HPLC).[1,2] The CEC technique can be defined as a type of capillary electrophoresis carried out in packed capillary columns in an environment in which an applied electric field is responsible for the movement of the mobile phase across the capillary, generating the electrosmotic flow (EOF).[3] Different from separations in zone capillary electrophoresis, the use of the stationary phase results in the separation of uncharged sample components. The major advantage of CEC compared to HPLC is the possibility of obtaining highly efficient columns while requiring smaller amounts of sample and mobile phase.[4] The high efficiency obtained with the use of the CEC technique is due to the EOF profile, that is different of the profile achieved by the pressure application, occurred at the HPLC technique.
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