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The development of new strategies and methodologies to directly, selectively, and sensitively record chemical signals of neurons involved in brain functions has drawn more and more attention because recording of the dynamic change of chemical signals affords a platform to understanding the chemical essence involved in various brain functions, for example, neurotransmission and the diagnosis and therapy of diseases. However, the chemical and physiological complexity of the central nervous system (CNS) makes the development of analytical methods for such a purpose very challenging. Our recent efforts on the development of new mechanisms for quantitative in vivo monitoring of brain chemistry have been based on the utilization of nanostructures to rationally create functional the electrode/electrolyte interface and carefully build surface chemistry of nanoparticles with specific surface/interface.