Multiclass method for the determination of pharmaceuticals and personal care products in compost from sewage sludge using ultrasound and salt-assisted liquid-liquid extraction followed by ultrahigh performance liquid chromatography-tandem mass spectrometry analysis

An analytical method for the analysis of 16 pharmaceuticals and personal care products in compost from sewage sludge is successfully validated. Ultrasound assisted extraction with a mixture of acetonitrile:ethyl acetate (1:1, v/v) containing 10% (v/v) of acetic acid was carried out. Two cycles of extraction of 10 min were applied. A clean-up of the extracts using salt-assisted liquid-liquid extraction (SALLE) was also included. Experimental design was used for the optimization of the main parameters involved in the extraction and cleaned-up steps. The chromatographic separation was carried out by ultrahigh performance liquid chromatography using a mobile phase gradient mixture of a 13 mM buffer ammonium formate solution (pH 9.25) (solvent A) and methanol (solvent B). An ACQUITY UPLC (R) BEH C18 column (1.7 mu m; 2.1 x 50 mm) column was used. Analytes were separated in less than 11 min. The compounds were detected and quantified using single reaction monitoring electrospray tandem mass spectrometry. The limits of detection calculated ranged from 0.5 to 4ngg(-1) d.w., and the limits of quantification from 2 to 13 ngg(-1) d.w. Recoveries from 93% to 111%, with relative standar deviations lower than 11% in all cases, were obtained. The method was applied to natural compost samples. High concentrations of some analytes were found. Ketoprofen (510 ngg-1 d.w.), methylparaben (240 ngg-1 d.w.), diclofenac (175 ngg-1 d.w.) and flufenamic acid (128 ngg-1 d.w.) were the most abundant. (C) 2017 Elsevier B.V. All rights reserved.