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

摘要： 为了探索经济适用的氟喹诺酮类残留提取和检测方法，建立了同时测定牛奶中6种氟喹诺酮类药物残留的高效液相色谱（HPLC ）串联荧光检测器（FLD）检测方法。样品经过含有5%乙酸的乙腈溶液涡旋提取，经改良QuEChERS方法净化，HPLC-FLD检测， 激发波长280 nm，发射波长450 nm，色谱柱为Waters XBridgeTM-C18柱（4.6 mm×250 mm，5 μm），流速1.0 mL/min，柱温 30℃，以乙腈和含0.1%甲酸的20 mmol/L甲酸铵水溶液做为流动相进行梯度洗脱。在所建立的方法中6种氟喹诺酮分离度较好（ R>1.5），在0.01～0.3 μg/mL浓度范围内具有良好的关系(r=0.999 9)，检出限在0.97～3.91 μg/kg之间，回收率试验中平 均加标回收率为97%～100%;重复性、精密度、稳定性试验结果良好，相对标准偏差均<3%。所建立方法简单、快速、灵敏度和 回收率高，适用于牛奶中该6种氟喹诺酮类药物残留的大批量筛选和定量测定。

关键词: HPLC-FLD, 牛奶, 氟喹诺酮类, 药物残留