高效液相色谱-荧光检测法对动物源性食品中氟喹诺酮类药物残留的检测

Determination of Fluoroquinolones Residues in Animal-Derived Products by High Performance Liquid Chromatography-Fluorescence

为了检测动物源性食品中氟喹诺酮类药物(沙拉沙星、环丙沙星、恩诺沙星)的残留量,本文对高效液相色谱-荧光检测法进行了优化。样品经无水硫酸钠除水,酸化乙腈提取,乙腈饱和的正己烷脱脂,采用0.05 mol/L的磷酸溶液(三乙胺调pH至2.4)-乙腈流动相进行复溶。结果表明,3种氟喹诺酮类药物在5~300 ng/mL呈现良好的线性关系,相关系数均大于0.999;在4~80μg/kg的加标浓度下,回收率为62.80%~94.45%,相对标准偏差为0.29%~5.30%。表明方法适用于动物源性食品中氟喹诺酮类药物残留量的检测。

In order to detect the residues of fluoroquinolones including sarafloxacin,ciprofloxacin and enrofloxacin in animal-derived products,the HPLC-FLD method was optimized.Samples were dewatered by anhydrous sodium sulfate,extracted with acidified acetonitrile,degreased with acetonitrile-saturated n-hexane,and reconstituted with 0.05 mol/L phosphoric acid solution(adjusted to pH=2.4 with triethylamine)-acetonitrile mobile phase.The results showed good linearities over the range of 5~300 ng/mL for three fluoroquinolones with good correlation coefficients(r2≥0.999).The recoveries were 62.80%~94.45%with relativestandard deviations in the range of 0.29%~5.30%at 4~80μg/kg spiked concentration.This method was suitable for the determination of fluoroquinolones residues in animal derived foods.