A high-performance liquid chromatography with fluorescence detection (HPLC–FLD) procedure was developed and refined to detect florfenicol (FF), its metabolite florfenicol amine (FFA), and three fluoroquinolone (FQ) residues present in poultry muscles concurrently. Sample pretreatment was conducted through liquid–liquid extraction (LLE). Ethylenediaminetetraacetic acid (EDTA), 90 % acetonitrile and acetonitrile were used as extraction solvents. The stationary phase employed was an XBridge BEH C18 column (5 μm, 4.6 mm × 150 mm), and the mobile phase consisted of a 0.01 mol/L solution of sodium dihydrogen phosphate and acetonitrile (65:35, V/V); the former contained 0.005 mol/L sodium dodecyl sulfate and 0.1 % triethylamine (pH adjusted to 4.8 with phosphoric acid). The limits of detection (LODs) and limits of quantification (LOQs) were 0.03–1.5 µg/kg and 0.1–5.0 μg/kg, respectively. The linear relationships were satisfactory within the corresponding concentration ranges, with determination coefficients (R2) ≥ 0.9997. The mean recoveries ranged from 70.34 to 94.98 %, and the intraday relative standard deviations (RSDs) and interday RSDs were 1.46–6.24 % and 1.60–7.31 %, respectively. This verified method is applicable and reliable for analyzing actual samples.
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