关键词: 超高效合相色谱；氟苯尼考；鱼肉；对映体；手性分离

Abstract: An ultra-performance convergence chromatography (UPC2) method was established for the separation and determination of the residues of florfenicol enantiomers and its metabolite florfenicol amine in fish meat. The samples were extracted with alkalized ethyl acetate, purified on a solid phase extraction column (MCX), and separated on a CHIRALPAK AD-3 column (150 mm × 3.0 mm, 3 μm) by gradient elution using a mobile phase consisting of supercritical CO2 (A) and aqueous ammonia-methanol in water (0.5:99.5, V/V) (B). The system’s back pressure and the column temperature were set at 13.8 MPa and 40 ℃, respectively. The linear correlation coefficients were greater than 0.999 3 in the range of 1.0–20.0 mg/L for the two florfenicol enantiomers and 2.0–40.0 mg/L for florfenicol amine, and the limits of quantification (RSN = 10) were 0.1 and 0.2 mg/kg, respectively. The recoveries of the florfenicol enantiomers and florfenicol amine from spiked fish in the range of 0.1–1.0 mg/kg were 81.5%–108.0%, with relative standard deviations (RSDs) of 5.3%–9.3%. This method is suitable for the separation and determination of the residues of florfenicol enantiomers and its metabolite in fish meat.

Key words: ultra-performance convergence chromatography; florfenicol; fish meat; enantiomer; chiral separation