Simple and rapid determination of 5-nitroimidazoles and metabolites in fish roe samples by salting-out assisted liquid-liquid extraction and UHPLC-MS/MS Hernández Mesa, Maykel Cruces Blanco, María Carmen García Campaña, Ana María 5-Nitroimidazoles Fish roe samples Salting-out assisted liquid-liquid extraction Ultra-high performance liquid chromatography Mass spectrometry 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. 2025-01-27T08:02:04Z 2025-01-27T08:02:04Z 2018-02-23 journal article https://hdl.handle.net/10481/100390 10.1016/j.foodchem.2018.01.101 eng http://creativecommons.org/licenses/by-nc-nd/4.0/ open access Attribution-NonCommercial-NoDerivatives 4.0 Internacional