Quantitative determination of octylphenol , nonylphenol , alkylphenol 1 ethoxylates and alcohol ethoxylates by pressurized liquid extraction and 2 liquid chromatography - mass spectrometry in soils treated with sewage 3 sludges 4 5

13 14 Surfactants have one of the highest production rates of all organic chemicals. Non-ionic 15 surfactants, especially alkylphenol ethoxylates, received most attention as precursors of 16 estrogenic metabolic products generated during wastewater treatment. Alkylphenols (octyl 17 and nonylphenol), alkylphenol polyethoxylates (APEOs), and alcohol ethoxylates (AEOs) 18 have been determined in a Mediterranean forest soil (Mediterranean Rendzic Leptosol) 19 amended with sludges from six waste water treatment plants (WWTPs) located in the 20 Valencian Community. These compounds were isolated from soil by pressurized liquid 21 extraction (PLE) using a mixture acetone-hexane (50:50 v/v), the extracts were cleaned up by 22 solid-phase extraction (SPE) with C18, and determined by liquid chromatography atmospheric 23 pressure chemical ionization-mass spectrometry (LC-APCI-MS) using analytical standards 24 for quantification. The method enabled high-reliable identification by monitoring the 25 corresponding ammonium adduct [M+NH3] for AEOs and APEOs, and the deprotonated 26 molecule [M-H] for octyl and nonylphenol. Recoveries, determined spiking soil samples at 27 different concentrations, ranged from 89 to 94 %, with limits of quantification from 1 to 100 28 μg kg. Data obtained from a soil sample mixed with biosolids in the laboratory showed that 29 these compounds are present at concentrations ranging from 0.02 to 5 mg kg. According to 30 these concentrations, levels of possible risk can be concluded for the presence of non-ionic 31 surfactant in soil. However, further assessment will be necessary to establish the relation-ship 32 between exposure and effect findings. 33 34