动物性食品中喹诺酮类抗生素残留测定

Determination of quinolones antibiotics residues in animal edible products

目的建立一种准确、快速、灵敏,能同时测定动物性食品中氧氟沙星、环丙沙星、恩诺沙星3种喹诺酮类(QNs)抗生素残留的方法。方法样品匀质后加入酸化乙腈,超声提取,用正己烷萃取除去杂质,乙腈层浓缩后,加入乙腈-水(8∶2)溶解残渣,采用高效液相色谱-紫外检测法检测。流动相为乙腈+0.01 mol/L磷酸二氢钠溶液(pH=4.0),采用梯度洗脱,检测波长279 nm。结果氧氟沙星、环丙沙星和恩诺沙星色谱图分离良好,峰形尖锐对称,相关系数均>0.999 6;3种不同加标浓度的氧氟沙星、环丙沙星、恩诺沙星相对标准偏差均<5%,重现性好,加标回收率均>85%;氧氟沙星、环丙沙星、恩诺沙星检测限分别为2.7×10-3、1.4×10-3、6.5×10-4μg/mL。结论高效液相色谱-紫外检测法快速、准确,可满足动物食品中3种QNs类抗生素残留的同时批量检测。

Objective To establish an accurate,rapid,and sensitive method for simultaneous detection of three quinolones（QNs） including ofloxacin（OFL）,ciprofloxacin（CIP）,and enrofloxacin（ENR）residues in animal edible products.Methods The residues in the samples were extracted by acidified acetonitrile（ACN）and ultrasonic wave device,and then the impurities were removed by liquid-liquid extraction（LLE）with hexane.After concentrated,the residues were dissolved by ACN-water（8：2）and then determined with high-performance liquid chromatograply-ultraviolate-visible detector（HPLC-UVD）.The mobile phase was ACN and sodium dihydrogen phosphate solution（0.01mol/L,pH=4.0）;gradient elution was used and the detection wavelength was 279 nm.Results OFL,CIP and ENR were seperated succssfully and the chromatographic peaks were sharp and symmetrical.The correlation coefficients were all above 0.999 6.The relative standard deviations of OFL,CIP,and ENR were all below 5%,with good reproducibilities.The recovery rates were all more than 85%.The limit of determination（LOD）of OFL,CIP,and ENR was 2.7＆times;10-3 μg/ml,1.4＆times;10-3 μg/ml,and 6.5＆times;10-4 μg/ml,respectively.Conclusion The method established is suitable for rapid,accurate,and simultaneous detection of OFL,CIP,and ENR in animal edible prodults.