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This digital document is a journal article from Analytica Chimica Acta, published by Elsevier in . The article is delivered in HTML format and is available in your Amazon.com Media Library immediately after purchase. You can view it with any web browser. Description: This work examines in deep the analytical performance of an example of ''first-generation'' microdevices: capillary electrophoresis microchip (CE) with end-channel electrochemical detection (ED). A hydroquinone and arbutin separation strategically chosen as route involving pharmaceutical-clinical testing, public safety and food control scenes was carried out. The reproducibility of the unpinched electrokinetic protocol was carefully studied and the technical possibility of working indiscriminately and/or sequentially with both simple cross-injectors was also demonstrated using a real sample (R.S.D.'s less than 7%). The robustness of the injection protocol allowed checking the state of the microchip/detector coupling and following the extraction efficiency of the analyte from real sample. Separation variables such as pH, ionic strength and, separation voltage were also carefully assayed and optimized. Analyte screening was performed using borate buffer (pH 9, 60mM) in less than 180s in the samples studied improving dramatically the analysis times used for the same analytes on a conventional scale (15min), with good precision (R.S.D.'s ranging 5-10%), accuracy (recoveries ranging 90-110%) and acceptable resolution (Rs>=1.0). In addition, the excellent analytical performance of the overall analytical method indicated the quality of the whole analytical microsystem and allowed to introduce the definition of robustness for methodologies developed into the ''lab-on-a-chip'' scene.