An integrated microdevice was utilized for the autonomous coupling of solid-phase extraction (SPE) to micellar electrokinetic chromatography (MEKC). Porous plugs of polymethacrylate polymer (similar to 200 mu m in length) were fabricated by ultraviolet irradiation in microchannels. Microcolumns of hydrophobic beads packed against the polymethacrylate plugs were utilized for the quantitative extraction of rhodamine B, yielding preconcentration factors over 200 for a 90-s extraction. The calculated detection limit for this dye was 60 M. A sample of coumarin dyes were concentrated by SPE, eluted in a nonaqueous solvent from a separate on-chip reservoir, and injected by a gated valve onto a separate column for MEKC analysis. Using the integrated device, a completely automated sequence of extraction, elution, injection, separation, and detection were performed in less than 5 min. Observed separation efficiencies were high, with plate heights below 2 mu m. The analysis was at least 3 times faster than semiautomated, conventional, solid-phase extraction, while requiring no user intervention. The design, fabrication, and autonomous operation of the device is discussed.