高效液相色谱法测定鸡肉中的氟喹诺酮类药物

Determination of Four Fluoroquinolone Residues in Chicken by High Performance Liquid Chromatography

建立鸡肉中4种喹诺酮类药物的HPLC-FLD检测方法。鸡肉样品经过无水硫酸钠脱水后用酸化乙腈提取,用乙腈饱和的正己烷除去杂质,下层乙腈液经氮气吹干后用流动相定容,再加入乙腈饱和的正己烷,混匀后在高速离心机上离心,下层液体用于高效液相色谱分析。采用Xbridge C18柱分离,以乙腈-磷酸二氢钠为流动相等度洗脱,荧光检测器检测,外标法定量。4种喹诺酮类药物标准曲线的线性回归系数均在0.999以上,线性范围为0.2～50μg/L,环丙沙星、恩诺沙星、沙拉沙星检出限为1.0μg/kg,达氟沙星检出限为0.3μg/kg。在20、40、80μg/kg添加水平下的添加回收为86.3%～102.3%,相对偏差为1.0%～4.6%。该方法具有快速,灵敏的特点,符合现行兽药残留分析的要求。

A simple, rapid, sensitive and reliable method was developed for analysis of four fluoroquinolone residues in chicken by HPLC-fluorescence detection （FLD）. Chicken samples were extracted with acetonitrile. Analytical separation was performed on Xbridge C18 Column with fluorescence detection. The mean recoveries of ciprofloxacin, ofloxacin, eurofloxacin and norfloxacin at the spiked levels of 20, 40, 80 mg/kg were between 80.3% and 102.3%.The relative standard deviations were between 1.0% and 4.6%. Linear range was 0.2-50 mg/L with the correlation coefficient being more than 0.999. The limits of detection for ciprofloxacin, enrofloxacin and norfloxacin were 1.0 μg/kg and the detection limit for ofloxacin was 0.3 μg/kg. This method is easy, fast, safe, sensitive and accurate, and can be used to simultaneously analyze residual quinolones in actual samples.