Automated method for the solid phase extraction of tetracyclines in wastewater followed by fluorimetric determination

Abstract

This work presents a multisyringe flow injection analysis (MSFIA) system for the automatic extraction and determination of tetracyclines in wastewater samples. The sample was adjusted with Na₂EDTA buffer before solid-phase extraction with an Oasis HLB column used for the analyte preconcentration. The europium (Eu³⁺)-based and citrate-mediated method (using Tris-HCl buffer) was selected for the fluorimetric analysis (λ_exc/em = 400/612 nm). For fluorescence detection, a low-cost system consisting of an USB 2000 CCD detector and a 3D-printed support that holds a LED light source was used. Under optimized conditions, the proposed method provided low limits of detection (9.4 μg L^-1) and quantification (31 μg L^-1), and good values for intra-day (<4 %) and inter-day precisions (<6 %). Recoveries of spiked TCs in wastewater samples ranged from 87 to 106 %. The results of this work were in good agreement with the measurements obtained by liquid chromatography coupled to a fluorescence detector.

Keywords: Automation; Fluorimetry; MSFIA; Solid-phase extraction; Tetracyclines; Wastewater analysis.