An efficient and eco-friendly injection-port tert-butyldimethylsilylated (TBDMS) derivatization and gas chromatography-mass spectrometry (GC-MS) was developed to determine triclosan (TCS, an antibacterial agent) in the samples of toothpaste, liquid hand-soap and facial cleansing cream. This on-line derivatization coupled ultrasonic extraction provides sensitivity, fast and reproducible results for TCS analysis. The accuracy and precision of the method was evaluated. The developed method was successfully applied to determine the content of TCS in selected personal care products.