This article presents a novel approach to capillary electrochromatography by which predetermined selectivity is achieved. A simple and quick method for the in situ preparation of monolithic molecularly imprinted flowthrough polymers inside fused silica capillaries is described. The superporous structure of the polymers permits rapid solvent and electrolyte exchange, as well as easy regeneration of the capillaries by hydrodynamic pumping. Chiral stationary phases were prepared by molecular imprinting of the β-adrenergic antagonists propranolol and metoprolol. The separation systems were operational within 3 h of the start of capillary preparation. Chiral separations with baseline resolution could be carried out in less than 120 s.

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Molecularly imprinted microparticles imprinted against (S)-propranolol were synthesised and studied for use in capillary electrochromatographic separation of propranolol enantiomers. The imprinted microparticles were in the size range of 0.2-0.5 micron as determined by scanning electron microscopy. The microparticles were suspended, in high concentration, in the electrolyte and used to perform enantiomer separation by a partial filling technique.

Three different capillary electrochromatographic methods for the enantiomer separation of beta-adrenergic antagonists (acebutolol, alprenolol, atenolol, metoprolol, pindolol, prenalterol, and propranolol) were applied using different cyclodextrins (beta-cyclodextrin, carboxymethyl-beta-cyclodextrin and dimethyl-beta-cyclodextrin) added to the electrolyte, a cross-linked protein-gel (cellobiohydrolase I) and a molecularly imprinted ((R)-enantiomer of propranolol) superporous polymer as chiral selectors. Through use of these different separation strategies, all the beta-adrenergic antagonists studied could be resolved into their enantiomers, although the three methods were carried out without extensive optimization. The protein and molecularly imprinted phases gave the highest selectivities whereas employing cyclodextrins resulted in the highest separation efficiency. Proteins and cyclodextrins are primarily natural products, albeit the cyclodextrins can be derivatized. In contrast, the molecularly imprinted chiral stationary phase can be highly customized when produced.

Molecularly imprinted polymer coatings were synthesized in fused-silica capillary columns by the use of a surface-coupled radical initiator. The coatings were prepared using either toluene, dichloromethane, or acetonitrile in the prepolymerization mixtures and were 0.15-2 microm thick as determined by scanning electron microscopy. Solvent-dependent differences in appearance were observed. All the molecularly imprinted polymer-based open-tubular capillary columns were able to separate the enantiomers of propranolol by means of electrochromatography. Electrochromatographic performance was found to be dependent on the type of solvent used during the synthesis.