Sequential superheated liquid extraction of pesticides, pharmaceutical and personal care products with different polarity from marine sediments followed by gas chromatography mass spectrometry detection

A method for the extraction of compounds with different polarity (namely, triclosan, estrone, 17β-estradiol, diethylstilbestrol, 4-octylphenol, procymidone, permethrin, oxyfluorfen, bisphenol A and 2,8-dibenzodichloro-p-dioxin) from marine sediments has been proposed. The proposed method consists of a sequential superheated fluid extraction with dichloromethane in a dynamic manner and with water in a static-dynamic manner for 50 min. The organic and aqueous extracts are independently collected and treated by evaporation and liquid-liquid extraction, respectively. The working conditions were optimized using multivariate approaches. Triclosan, bisphenol A, oxyfluorfen and permethrin were quantitatively extracted with repeatability and reproducibility in the range 2.9-9.1 and 5.5-9.1% R.S.D., respectively. The analytes were identified and quantified by gas chromatography-tandem mass spectrometry. The method was compared with conventional Soxhlet for the extraction of the analytes from spiked (at low ppb levels) sediments collected at the outflow of an urban wastewater treatment plant and non-spiked sediment collected from a sporting harbour. Statistical differences between the results of both methods were not found from the t-test for 95% of confidence level (p-value = 0.131).