高效液相色谱法检测鸡肉中氟喹诺酮类药物残留量前处理方法的优化

    An optimization study on determination of fluoroquinolones residues in chicken muscle by high performance liquid chromatography

    • 摘要: 【目的】建立一种用高效液相色谱法快速检测鸡肉组织中5种氟喹诺酮类药物(诺氟沙星、环丙沙星、达氟沙星、恩诺沙星、沙拉沙星)残留量的方法.【方法】样品的提取液由乙腈与三氯乙酸溶液(质量分数2%)按体积比 1∶3 的比例混合而成,流动相为乙腈-磷酸/三乙胺溶液(0.02 mol·L-1),荧光激发波长280 nm,发射波长450 nm.【结果和结论】添加低、中、高浓度水平时,回收率为84.71%~99.66%,变异系数为0.20%~4.34%.该方法检测诺氟沙星、环丙沙星和恩诺沙星的残留定量限为10 μg·kg-1,达氟沙星的残留定量限为2 μg·kg-1,沙拉沙星的残留定量限为20 μg·kg-1.此法操作简单、实用,灵敏度高,可以满足鸡肉食品中氟喹诺酮类药物残留检测的需要.

       

      Abstract: 【Objective】A method for rapid determination of five fluoroquinolones (norfloxacin,ciprofloxacin,danofloxacin,enrofloxacin,sarafloxacin) residues in chicken muscle using high performance liquid chromatography (HPLC) was established.【Method】The extracting solution of the chicken samples included a mixture of acetonitrile and trichloroacetic acid(the mass fraction of 2%). HPLC mobile phase consisted of acetonitrile and phosphate buffer (0.02 mol·L-1) with triethy lamine. Fluorometric excitation wavelength was 280 nm, and emission wavelength was 450 nm. 【Result and conclusion】The recoveries of 5 fluoroquinolones were 84.71%-99.66% at three spiked level(low, medium, high), and the relative standard deviations (RSD) were 0.20%-4.34%.The limit of quantiation (LOQ) of norfloxacin, ciprofloxacin and enrofloxacin was 10 μg·kg-1. The LOQ of danofloxacin was 2 μg·kg-1, and the sarafloxacin was 20 μg·kg-1. The method is simple, practical, and sensitive. It can meet the needs of determination of fluoroquinolones in chicken muscle.

       

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