Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Av. Fuentenueva s/n, E-18071 Granada, Spain.
Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Av. Fuentenueva s/n, E-18071 Granada, Spain.
Food Chem. 2018 Jun 30;252:294-302. doi: 10.1016/j.foodchem.2018.01.101.
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 (R ≥ 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.
提出了一种新的多残留方法，用于使用 UHPLC-MS/MS 测定鱼卵样品中的 12 种 5-硝基咪唑类化合物及其代谢物。在样品分析前进行了加盐辅助液-液萃取程序。化合物的分离在 25°C 下使用 C18 Zorbax Eclipse Plus 柱（50mm×2.1mm，1.8μm）和由 0.025%（v/v）甲酸水溶液和纯 MeOH 组成的流动相在 0.5mL/min 的流速下完成。还优化了离子化和碎裂参数。该方法的线性（R≥0.9992）、提取效率（≥68.9%）、重复性（RSD≤9.8%）、重现性（RSD≤13.9%）和准确性（回收率≥81.4%）进行了特征描述。决策限（CCα）和检测能力（CCβ）分别在 0.1-1.0 和 0.2-1.7μg/kg 的范围内获得。
