关键词: HPLC-FLD, 牛奶, 氟喹诺酮类, 药物残留

Abstract: In order to develop a high performance liquid chromatography, high performance liquid chromatography series fluorescence detector (HPLC-FLD) detection method was established, which could detected 6 fluoroquinolones residues in milk at the same time. The sample after acetonitrile containing 5% acetic acid extraction of the vortex, the modified QuEChERS method of HPLC-FLD purification, detection, excitation wavelength 280 nm and emission wavelength of 450 nm, the column was Waters XBridgeTM-C18 column (4.6 mm×250 mm,5 μm), the flow rate of 1 mL/min, the column temperature of 30℃, with acetonitrile and 0.1% formic acid. 20 mmol/L ammonium formate solution as mobile phase gradient elution. In the method of good separation of 6 fluoroquinolones (R>1.5), in 0.01~0.3 g/mL concentration range with good relationship (r=0.999 9), the detection limit is between 0.97~3.91 g/kg, the recovery rate of test in the average recovery rate was 97%~100%. Repeatability, precision, stability test results are good, the relative standard deviation are <3%. The established method is simple, rapid, sensitive and high recovery rate, suitable for mass screening and quantitative determination of 6 kinds of fluoroquinolones residue in milk.

Key words: HPLC-FLD, milk, fluoroquinolones, drug residues