Three microbore liquid chromatography (LC) assays for determination of amino acids in rat brain dialysates are described: one for separation of amino acids by gradient elution and electrochemical detection, one for analysis of GABA by isocratic elution and electrochemical detection, and one for fast measurement of glutamate and aspartate by gradient elution and fluorescence detection. The assays are reliable, reproducible and sensitive. In comparison with conventional LC, a 5-fold increase in sensitivity was obtained for GABA. Optimization of the derivatization chemistry and the microbore LC system are discussed, as well as important practical aspects.