Determination of polycyclic aromatic hydrocarbons, phthalate esters, alkylphenols and alkyphenol ethoxylates in sediment using simultaneous focused ultrasound solid–liquid extraction and dispersive solid-phase extraction clean-up followed by liquid chromatography

Abstract

The study presents a simple and non-laborious method for the determination of 16 polycyclic aromatic hydrocarbons (PAHs), 2 phthalate esters (PEs), 2 alkylphenols (APs) and 4 alkylphenol ethoxylates (APEOs) in sediment. The method employs sample preparation combining focused ultrasound solid–liquid extraction (FUSLE) and in situ clean-up followed by liquid chromatography with fluorescence and ultraviolet detection. Extraction of 0.5 g sediment samples with 7 mL acetone in the presence of activated silica (0.5 g) and powdered copper (0.2 g) using an ultrasonic probe for 1 min resulted in recoveries of target analytes ≥ 78 %. The analytical method was classified as “acceptable green analysis” by the analytical Eco-Scale assessment (AESA) and scored 0.54 in the AGREEprep greenness assessment for sample preparation. Matrix-matched calibration was used to quantify analytes with a linear range for PAHs 2–1000 ng g–1, for PEs 100–5000 ng g–1 and for APs and APEOs 40–2000 ng g–1 dry weight. The reached limits of quantification (LOQ) for PAHs ranged from 1.1 to 3.1 ng g−1, for PEs from 122 to 124 ng g−1, for APs from 40 to 51 ng g−1 and for APEOs from 36 to 53 ng g−1. The applicability of the method was demonstrated by the analysis of real sediment samples and natural matrix certified reference material.