高效液相色谱法快速测定鸡蛋中5种氟喹诺酮类药物残留

Rapid Determination of Five Fluoroquinolones in Eggs by High Performance Liquid Chromatography

建立了一种检测鸡蛋中环丙沙星、达氟沙星、恩诺沙星、二氟沙星及沙拉沙星残留的高效液相色谱方法。该方法前处理简便快速,样品经低浓度乙腈结合加热促使蛋白质快速沉淀,正己烷脱脂,分离清液后进高效液相色谱仪分析。流动相为0.05 mol/L磷酸/三乙胺溶液-乙腈溶液(80∶20),荧光检测器的激发波长为280 nm,发射波长为450 nm。该方法对环丙沙星和二氟沙星的定量下限为5μg/kg,达氟沙星的定量下限为0.5μg/kg,恩诺沙星的定量下限为2.5μg/kg,沙拉沙星的定量下限为10μg/kg。在定量下限及低、中、高4种加标浓度下,5种氟喹诺酮类药物的平均回收率为92.2%~107.1%,批内相对标准偏差(RSD)为0.6%~5.8%,批间相对标准偏差为1.5%~5.0%。方法具有前处理简单、环保、快捷、准确度和灵敏度高等优点,适合生产线和流通环节鸡蛋样品的快速检测。

A high performance liquid chromatography（HPLC） method combined with a rapid and simple pretreatment approach was established for the determination of five fluoroquinolones（ciprofloxacin,danofloxacin,enrofloxacin,difloxacinand and sarafloxacin） residues in eggs. Samples were extracted with acetonitrile. Protein in egg samples was precipitated by heating in water-bath. The supernatants were degreased with n-hexane,and followed by HPLC analysis. The mobile phase consisted of 0. 05 mol/L phosphoric acid and triethylamine-acetonitrile（80 ∶ 20）. The fluorometric excitation wavelength was 280 nm,and the emission wavelength was 450 nm. The limits of quantitation（LOQ） for ciprofloxacin,difloxacin,danofloxacin,enrofloxacin and sarafloxacin were 5,5,0. 5,2. 5 and 10 μg/kg,respectively. The average recoveries for 5 fluoroquinolones were in the range of92. 2%-107. 1% at four spiked levels（LOQ,2 LOQ,4 LOQ and 20 LOQ）,and the intra-day and inter-day relative standard deviations（RSDs） were in the ranges of 0. 6%-5. 8% and 1. 5%-5. 0%,respectively. The proposed method is rapid, accurate, sensitive and eco-friendly, and could be used for the quick analysis on residues of fluoroquinolones in egg in its production and distribution for consumption.