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Chemical separation remains a core tool in the arsenal of analytical chemists involved in anything from biological research to pharmaceutical industry to environmental analysis. The continued evolution of separation methods such as chromatography and electrophoresis is driven by the need for a fast analysis of complex mixtures on a smaller scale. At AMPRI, activities have been aimed at developing new analytical methods and applications of electrophoresis & chromatography. This involves techniques for the separation of toxicants, pharmaceuticals and biomolecules and their detection at ppb level using miniaturized separation techniques i.e. high performance liquid chromatography, capillary electrophoresis, miceller electrokinetic chromatography, microchip based electrophoresis and gas chromatography techniques coupled with UV-Vis spectrophotometry, fluorescence, laser indused fluorescence, electrochemical and mass spectrophotometric detection. Emphasis has also been laid in this case on miniaturizing separation methods so that analysis can be performed on extremely small samples, i.e., “lab-on-a-chip” systems. Studies to increase the speed of separation analysis to sub-second levels for rapid, high-throughput analysis and interfacing separations to a variety of detectors are ongoing. Applications to a variety of topics including metabolomics, proteomics, neuroscience, toxicants and pharmaceuticals are being explored. Further, the applications of microfluidics are among the greatest engineering challenges of the century and include the realization of optimized processes in mixing, reaction, separation, pre-concentration, and detection of chemical species. The focus in this context is on the development of new detection tools for separation matrices and analytical principles for miniaturized separation system and development.