Determining the distribution of triclosan and methyl triclosan in estuarine settings

We have developed a method for the analysis of two sewage-derived contaminants: triclosan (TCS), an antibacterial agent, and methyl triclosan (MTCS), a TCS metabolite. For solid samples (4 g), extraction and cleanup were integrated into the same step using pressurized liquid extraction (PLE) with in-cell-clean-up (1 g of florisil). The extraction was performed using dichloromethane at 100 °C, 1500 psi and 3 static extraction cycles of 5 min each. For water samples (100 mL), stir bar sorptive extraction-liquid desorption (SBSE-LD) was used. Bars were stirred for 10 h and analytes were later desorbed using acetonitrile. Finally, MTCS and a silylated derivative of TCS were determined by gas chromatography-mass spectrometry (GC-MS). Recovery experiments in water and sediments were performed and the results ranged from 67% to 78%. Limits of detection (LODs) were 5 ng L−1 for TCS and 1 ng L−1 for MTCS, in water samples, and 0.1 ng g−1 for TCS and MTCS in solid samples. The method was applied then to determine the levels of these compounds in the estuary of Guadalete River (SW Spain). TCS and MTCS concentrations up to 9.6 ng g−1 in sediments and 310 ng L−1 in water were measured. Their distribution was strongly influenced by the presence of wastewater sources, treated and untreated, along the sampling area, where maximum concentrations were detected. Highest values were reached in the water column during low tides as the water volume in the estuary becomes lower.