A validated reverse-phase HPLC-DAD for the simultaneous determination of triclosan and triclocarban in surface water has been developed, because this method has not been used for determination of these disinfectant agents so far. An isocratic elution was achieved using a Develosil RP Aqueous AR-5 RP-30 column with a flow rate of 1.0 mL min−1. The mobile phase consisted of mixed methanol and water in raito of 90:10, v/v. DAD detector was used to monitor the analytes at 280 nm for triclosan and 265 nm for triclocarban. The time of analysis was 10 min and the retention time for triclosan and triclocarban was 5.81 min and 8.13 min, respectively. The solid phase extraction method was proposed for the preconcentration step. The extraction efficiencies were approximately 97% for triclosan and 87% for triclocarban. The linearity range for triclosan and triclocarban after pre-concentration were between 0.5–20 μg mL−1 and 0.3–20 μg mL−1, respectively. The LOD and LOQ of triclosan and triclocarban in real samples were 0.04 ng mL−1 and 0.11 ng mL−1, 0.17 ng mL−1 and 0.50 ng mL−1, respectively. The method has been sensitive and can be successfully applied to the fast and simultaneous determination of triclosan and triclocarban in surface waters.