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Peroxodisulfate as a chemical initiator for methacrylate‐ester monolithic columns for capillary electrochromatography
Author(s) -
CantóMirapeix Amparo,
HerreroMartínez Jose M.,
Benavente David,
MongayFernández Carlos,
SimóAlfonso Ernesto F.
Publication year - 2008
Publication title -
electrophoresis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.666
H-Index - 158
eISSN - 1522-2683
pISSN - 0173-0835
DOI - 10.1002/elps.200700458
Subject(s) - azobisisobutyronitrile , chemistry , capillary electrochromatography , polymerization , monolithic hplc column , methacrylate , solvent , chromatography , polymer chemistry , stationary phase , polymer , organic chemistry
Organic monolithic stationary phases for CEC were synthesized in situ in fused‐silica capillaries. Polymerization mixtures were composed of butyl methacrylate, ethylene dimethacrylate, and [2‐(methacryloyloxy)ethyl]trimethyl ammonium chloride in the presence of a porogenic solvent, using ammonium peroxodisulfate as chemical initiator, and N , N , N ′, N ′‐tetramethylethylenediamine to activate the reaction. The influence of the amount of initiator, temperature, and composition of porogenic solvent on the physical and chromatographic properties of monolithic stationary phases has been investigated. A minimum plate height of 14.5 μm was obtained at 18 wt% of 1,4‐butanediol in the polymerization mixture. The produced monolithic stationary phases exhibited a good repeatability and batch‐to‐batch and mixture‐to‐mixture reproducibility, with RSD values below 5.6% in the electrochromatographic parameters studied. A comparison with columns prepared by thermal initiation with α,α′‐azobisisobutyronitrile (AIBN) was also performed. The most efficient column initiated with peroxodisulfate showed better efficiencies and selectivities than that prepared with AIBN at the same composition mixture.