Ultra-high performance liquid chromatography with fluorescence detection following salting-out assisted liquid–liquid extraction for the analysis of benzimidazole residues in farm fish samples

  • Acknowledgements: The authors gratefully acknowledge the financial support of the Andalusian Government (Junta de Andalucía) for supporting this work (Excellence Project Ref: P12-AGR-1647) and Spanish Ministry of Economy and Competitiveness (Project ref: AGL2015-70708-R). CTC thanks to the Excellence Project Ref: P12-AGR-1647 for a predoctoral fellowship. FJL is grateful for postdoctoral personal funding through the Special Research Program of the University of Granada.
  • Authors: C. Tejada-Casado, F.J. Lara, A.M. García-Campaña, M. del Olmo-Iruela.
  • Reference: Journal of Chromatography A 1543 (2018) 58-66.

Ultra-high performance liquid chromatography (UHPLC) coupled with fluorescence detection (FL) has been proposed for the first time to determine thirteen benzimidazoles (BZs) in farmed fish samples. In order to optimize the chromatographic separation, parameters such as mobile phase composition and flow rate were carefully studied, establishing a gradient mode with a mobile phase consisted of water (solvent A) and acetonitrile (solvent B) at a flow rate of 0.4 mL/min. The separation was performed on a Zorbax Eclipse Plus RRHD C18 column (50 × 2.1 mm, 1.8 μm), involving a total analysis time lower than 12 min. Salting-out assisted liquid-liquid extraction (SALLE) was applied as sample treatment to different types of farmed fish (trout, sea bream and sea bass). To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized including the amount of sample, type and volume of the extraction solvent, and the nature and amount of the salt used. Characterization of the method in terms of performance characteristics was carried out, obtaining satisfactory results for the linearity (R2 ≥ 0.997), repeatability (RSD ≤ 6.1%), reproducibility (RSD ≤ 10.8%) and recoveries (R ≥ 79%; RSD ≤ 7.8%). Detection limits between 0.04–29.9 μg kg−1 were obtained, demonstrating the applicability of this fast, simple and environmentally friendly method.

This entry was posted in AGL2015-70708-R, Anthelmintic, Aquaculture products, Benzimidazoles, Fluorescence, P12-AGR-1647, SALLE, Sea bass, Sea bream, Trout, UHPLC and tagged , , . Bookmark the permalink.