Triclocarban (TCC) and triclosan (TCS) are used in a wide range of household and personal care products and have been the most frequently detected organic pollutants in both wastewater and surface water. This paper presented a rapid analytical method for simultaneous determination of TCC and TCS in wastewater. The method involves the extraction and cleanup of the target compounds by using silicon dioxide/polystyrene composite microspheres solid-phase extraction and detection with ultra-high-pressure liquid chromatography. Under the optimized conditions, the limits of detection were 0.028 μg/L and 0.040 μg/L for TCC and TCS, respectively. Under the concentrations of the spiking level ranging from 0.100 μg/L to 2.000 μg/L, the spiked recoveries of TCC and TCS in wastewater samples achieved in the range of 89.5–102.8% with RSD below 6.3% for TCC and 95.5–103.6% with RSD below 6.9% for TCS. This method was successfully used in monitoring the water samples from three traditional wastewater treatment plants.
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