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A method for the rapid determination of monoamine oxidase (MAO) activity by capillary electrophoresis (CE) has been established. The effect factors including the pH, the concentration of electroosmotic flow modifier (OFM), the salt concentration of running buffer were investigated in detail. The analysis was performed in an uncoated fused-silica capillary with 50 mum id and total length of 70 cm (40 cm to the detector ) under the applied voltage of 15KV with a running buffer of 50 mmol/L phosphate buffer saline (PBS) and 0.5 mmol/L tetradecyltrimethyl ammonium bromide (TTAB) (pH 10.5), detected by UV detector at 214nm. The linear range of 4-hydroxyyquinoline, which is the product of the MAO deaminated Kynuramine, between peak area and concentration was was from 10 mumol/L to 1 000 mumol/L, with correlation coefficient of 0. 9997. The precision of the method was below 8.5% ( n =5). The limit of detection was 2 mumol/L (S /N = 3).