Determination of sulfonamide residues in animal foodstuffs by magnetic dispersive solid-phase extraction using magnetic carbon nanocomposites coupled with ion pair-dispersive liquid–liquid micro-extraction combined with HPLC-DAD

Abstract

In this study, magnetic-dispersive solid-phase extraction coupled with ion pair-dispersive liquid–liquid micro-extraction (MSPE-i-DLLME) was used to the pre-concentration and extraction of five sulfonamides residues (sulfadiazine, sulfathiazole, sulfacetamide, sulfamethazine and sulfamethoxazole) in animal foodstuffs. The sulfonamides are extracted using magnetic carbon nanocomposite and then eluted with acetonitrile. In the DLLME step, the target analytes are collected in 1-octanol containing 10% Aliquat-336 (as extraction solvent). Finally, the compounds are quantified by HPLC with DAD detection. The extraction parameters optimized using the one at the time and central composite design methods. Under the optimized conditions: sample solution volume was 100 mL; initial pH: 12, amounts of MCNs: 30 mg; desorption solvent (ACN) volume, 1 mL; desorption condition, 10 min sonication at two step; extraction solvent (1-octanol + 10% aliquat) volume, 115 µL; pH of DLLME step, 3; salt effect, 24.6%, (w/v) NaCl; centrifuge, 5 min, 4000 rpm. In these extraction conditions, the proposed procedure represented good pre-concentration factors between 130 and 490; detection limits in the range from 0.01 to 5 μg kg−1 (at S/N = 3), and linear response in the 0.1–400 μg kg−1 concentration range. The method is successfully applied to the determination of sulfonamides residues in animal foodstuffs.