Polyrotaxane approach for synthesis of continuous beds for capillary electrochromatography

Abstract

The polyrotaxane formation approach was evaluated for synthesis of continuous beds for capillary electrochromatography. This approach has the advantage of generating diverse electroosmotic and chromatographic properties without chemical reactions. The polyrotaxane derivatized continuous beds were formed adding the macrocyclic compounds to the solution of neutral acrylic monomers and crosslinker prior to the initiation of the polymerisation. Cationic and anionic derivatives of β-cyclodextrin were used as macrocyclic compounds. Investigation of the electroosmotic properties indicated a template directed and enthalpy controlled self-assembly of the polyrotaxanes during the polymerisation of the continuous beds. This process was monomer-composition dependent and favored by the hydrophobicity of the polymeric skeleton. The morphology of the continuous beds was evaluated using high-resolution optical microscopy with CCD camera and atomic force microscopy. Reversed-phase capillary chromatography driven by electroosmosis, originating from the polyrotaxane structure, was performed using several test mixtures. Not primarily designed for the chiral chromatography the polyrotaxane derivatized continuous beds demonstrated enantioselective separation of d,l-metoprolol. The stability of the polyrotaxane derivatized continuous beds was tested. The beds demonstrated reproducible electroosmotic properties in the range from pH 4 to pH 9 (RSD=0.69%).