Continuous full filling capillary electrochromatography with nanoparticles as pseudostationary phase interfaced with electrospray ionisation mass spectrometric detection was used for reversed phase separations with very high separation efficiency. Several batches of nanoparticles were synthesised and their electrochromatographic performance were evaluated. Different parameters, such as repeatability, reproducibility, limit of detection, and peak asymmetry, were investigated yielding excellent results. The stability of the system over wide pH ranges and over time was found to be excellent. Very high separation efficiencies with over 1.1 million theoretical plates per metre were obtained. The limit of detection for the investigated dialkyl phthalates was approximately 1.0 μmol L-1, corresponding to 3-5 fmol injected. After preparation, nanoparticle suspensions could be used without further treatment for at least an entire working day with maintained chromatographic qualities. © 2007 Elsevier B.V. All rights reserved.
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