OBJECTIVE: To establish a method for the concentration determination of catecholamines in human urine. METHODS: After extracted by aluminum oxide, using 3, 4-dihydroxybenzylamine as internal standard, HPLC-electrochemistry was performed on the column of Shim-Pack C18 with mixed solution [every 500 ml mixed solution containing ion-pairing reagents (octane sulfonate) 0.5 mmol, methanol 10 ml, 0.06 mmol/L Di-n-butylamine 50 μl, sodium acetate anhydrous 2.0 g, citric acid 5.5 g, EDTA-Na2 60 mg and sodium chloride 584.4 mg, pH=3.5] at a flow rate of 0.8 ml/min, column temperature was 30 ℃, detection voltage was 750 mV, and injection volume was 40 μl. RESULTS: The linear ranges were 3.125-100 ng/ml for both norepinephrine (r=0.998 5) and epinephrine (r=0.999 2), lower limits of quantitation were 3.125 ng/ml; RSDs of within days and daytime were lower than 10%, method recoveries were 99.2%-101.6% and 98.9%-100.5%, extraction recoveries were 63.8%-66.8% and 60.5%-62.6%. CONCLUSIONS: The method shows strong specificity, high sensitivity and low detection cost, and can be used for the concentration determination of catecholamines in human urine.