ASE/UHPLC-FLD Determination of Florfenicol and Florfenicol Amine Residues in Pigeon and Quail Eggs

  Objective  To establish an analytical method for simultaneous detections of florfenicol (FF) and its metabolite, florfenicol amine (FFA), in animal-derived foods.

  Method  Samples of pigeon and quail eggs were extracted by the accelerated solvent extraction (ASE) method with acetonitrile-ammonia (98:2, V/V) as the solvent. The extract was degreased and purified with acetonitrile-saturated n-hexane. A mobile phase consisting of 0.005 mol·L⁻¹ NaH₂PO₄, 0.003 mol·L⁻¹ sodium lauryl sulfate and 0.05% trimethylamine was used in the ultra-high performance liquid chromatography-fluorescence (ASE/UPLC-FLD) determination of FF and FFA contents.

  Result  Highly correlated linear relationships (R²>0.999 2) within the limit of quantitation (LOQ) were achieved between the peak area and concentration on the target compounds. The average recoveries of the method at the spiked levels of 50.0, 100.0, 200.0 μg·kg⁻¹ and LOQ ranged from 84.69% to 98.04% with RSDs less than 3.7%. The method delivered the limit of detection (LOD) and LOQ on FF in the pigeon eggs at 4.8 µg·kg⁻¹ and 11.2 µg·kg⁻¹, respectively, and those on FFA, at 1.9 µg·kg⁻¹ and 4.8 µg·kg⁻¹, respectively; whereas, those on FF in the quail eggs, at 4.7 µg·kg⁻¹ and 10.6 µg·kg⁻¹, respectively, and those on FFA, at 1.8 µg·kg⁻¹ and 4.6 µg·kg⁻¹, respectively.

  Conclusion  The newly developed analytical methodology was rapid, simple, sensitive, and considered suitable for FF and FFA determinations in pigeon and quail eggs.