惠芸华, 沈晓盛, 冯兵, 于慧娟. 固相萃取-高效液相色谱法测定水产品中7种氟喹诺酮类药物残留[J]. 农药学学报, 2009, 11(4): 462-466.
    引用本文: 惠芸华, 沈晓盛, 冯兵, 于慧娟. 固相萃取-高效液相色谱法测定水产品中7种氟喹诺酮类药物残留[J]. 农药学学报, 2009, 11(4): 462-466.
    HUI Yun-hua, SHEN Xiao-sheng, FENG Bing, YU Hui-juan. Determination of Seven Fluoroquinolones Residue in AquaticProducts by Solid-phase Extraction-HPLC[J]. Chinese Journal of Pesticide Science, 2009, 11(4): 462-466.
    Citation: HUI Yun-hua, SHEN Xiao-sheng, FENG Bing, YU Hui-juan. Determination of Seven Fluoroquinolones Residue in AquaticProducts by Solid-phase Extraction-HPLC[J]. Chinese Journal of Pesticide Science, 2009, 11(4): 462-466.

    固相萃取-高效液相色谱法测定水产品中7种氟喹诺酮类药物残留

    Determination of Seven Fluoroquinolones Residue in AquaticProducts by Solid-phase Extraction-HPLC

    • 摘要: 建立了固相萃取-反相高效液相色谱法同时测定水产品(河鳗、南美白对虾和罗非鱼)中7种氟喹诺酮类药物残留的方法。样品经1 mol/L磷酸盐提取、正己烷去脂、C18固相萃取柱净化后,用高效液相色谱分离、荧光检测器检测、外标法定量。诺氟沙星、环丙沙星和恩诺沙星的最低添加水平为5.0 μg/kg,单诺沙星为1.0 μg/kg,培氟沙星为4.0 μg/kg,沙拉沙星为20.0 μg/kg,氧氟沙星为30.0 μg/kg。结果表明,7种氟喹诺酮类药物的平均回收率在75% ~95%之间,相对标准偏差为1.3% ~9.3%;检测限在0.07 ~5.84 μg/kg之间,定量限在0.23 ~19.48 μg/kg之间。采用所建立方法对上海农贸市场随机抽取的实际样品进行检测,结果均未检出7种氟喹诺酮类药物残留。

       

      Abstract: A reversed-phase HPLC method for analyzing seven fluoroquinolones residue in aquatic products (Anguilla anguilla,Penaeus vannamei and Oreochromis spp.) with fluorescence detector was developed.The fluoroquinolones residue was extracted by phosphate,purified with n-hexane and solid-phase extraction,quantified using external standard calibration method.The minimum added concentration was 5.0 μg/kg for norfloxacin,ciprofloxacin and enrofloxacin,1.0 μg/kg for danofloxacin,4.0 μg/kg for pefloxacin,20.0 μg/kg for sarafloxacin and 30.0 μg/kg for ofloxacin.The average recoveries of the seven fluoroquinolones in aquatic product ranged from 75% to 95%,with relative standard deviations of 1.3%- 9.3%.The limit of detection (LOD) was 0.07- 5.84 μg/kg, the limit of quantification (LOQ) was 0.23 -19.48 μg/kg.Samples obtained optionally from shanghai terminal market were analyzed with the established method,and no fluoroquinolone was detected.

       

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