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Two major approaches will be presented in this work.First, a novel integrated capillary electrochromatography (CEC)-electrospray ionization (ESI)-mass spectrometry (MS) micro-device with nanoflow was developed for the analysis of amino acids and peptides.Nafion tubing junction was employed in the ESI interface.Lupamin, a high molecular weight linear positively charged polyvinylamine polymer coated on the inner wall of open-tubular capillary generates strong electroosmotic flow for supporting a steady nanoelectrospray and works as the stationary phase for providing the chromatographic selectivity for resolving amino acids and peptides and minimizing analyte adsorption.The device is very reliable and reproducible for CEC-ESI-MS analysis of amino acids and peptides for over a hundred operations.