A fast method for determination of homocysteine and glutathione using an electrochemical microchip capillary electrophoresis which has several advantages, high efficiency (The detection limit for homocysteine and glutathione are 3.8 nM and 3.7 pM respectively.The linear range of detection is from 488.5 nM to 500 μM for homocysteine and from 61 nM to 250 μM for glutathione.), short time of analysis(less than 2 min). and small amounts of sample and buffer (50 – 200 μL ).The method was applied to theseparation and determination of glutathione in clinical medicine and homocysteine in human plasma.