Multiclass and multi-residue determination of pesticides and antibiotics in sediment from an aquacultural environment based on modified dispersive solid-phase extraction

Abstract

A quick, easy, cheap, effective, rugged, and safe method was developed for the multi-residue analysis of pesticides and antibiotics in aquaculture sediment using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The developed method is based on ultrasonic extraction with acetonitrile and phosphate buffer, salting with sodium chloride, and cleaning with dispersive solid-phase extraction adsorbent using primary secondary amine, C₁₈, and graphitized carbon black, followed by HPLC-MS/MS detection. We optimized different extraction methods and the ratio of the cleanup adsorbents to achieve good recoveries at three spiking levels that ranged from 60.4% to 114% with a relative standard deviation below 15% (n = 6). For all analytes, except for flufenoxuron, the limits of quantification were between 1 and 5 µg/kg (dry weight). The validated method was successfully applied to real samples collected from 20 aquacultural ponds, confirming the feasibility of the proposed method. The concentrations of the target analytes in the sediments (dry weight) were in the ranges of 2.2–35.0 µg/kg for sulfonamides, 0–409.1 µg/kg for quinolones, 0–6.56 µg/kg for macrolides, and 0–4.9 µg/kg for pesticides. Moreover, the co-occurrence of pesticides and antibiotics may potentially pose a high risk to sediment-dwelling organisms in nine out of the 20 investigated locations.