- Acknowledgements: The authors gratefully acknowledge the financial support of the “Junta de Andalucía” (Proyecto de Excelencia Ref: P12-AGR-1647). Maykel Hernández-Mesa thanks the Plan Propio of the University of Granada for a pre-doctoral contract.
- Authors: M. Hernández-Mesa, C. Cruces-Blanco, A.M. García-Campaña.
- Reference: Food Chemistry 252 (2018) 294–302.
A novel multiresidue method is proposed for the determination of 12 5-nitroimidazoles and their metabolites in fish roe samples using UHPLC-MS/MS. A salting-out assisted liquid-liquid extraction procedure was performed prior to sample analysis. The separation of compounds was accomplished using a C18 Zorbax Eclipse Plus column (50 mm × 2.1 mm, 1.8 µm) at 25 °C and a mobile phase consisting of 0.025% (v/v) aqueous formic acid and pure MeOH at a flow rate of 0.5 mL/min. Parameters involved in ionization and fragmentation were also optimized. The method was characterized in terms of linearity (R2 ≥ 0.9992), extraction efficiency (≥68.9%), repeatability (RSD ≤ 9.8%), reproducibility (RSD ≤ 13.9%) and trueness (recoveries ≥81.4%). Decision limits (CCα) and detection capabilities (CCβ) were obtained in the ranges 0.1–1.0 and 0.2–1.7 µg/kg, respectively.
