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当前位置: 首页 > 文章 > 高效液相色谱法同时测定水产品中6种喹诺酮药物的残留 食品科学 2010,31 (6) 185-189
Position: Home > Articles > High Performance Liquid Chromatographic Method for Simultaneous Determination of Six Quinolone Residues in Aquatic Products FOOD SCIENCE 2010,31 (6) 185-189

高效液相色谱法同时测定水产品中6种喹诺酮药物的残留

作  者：
钱卓真;苏秀华;魏博娟;吴成业
单  位：
福建省水产研究所;厦门大学材料学院;集美大学生物工程学院;福建农林大学食品科学学院
关键词：
反相高效液相色谱法;荧光色谱;喹诺酮类药物;多残留检测;水产品
摘  要：
建立用固相萃取-反相高效液相色谱法同时检测水产品中6种喹诺酮药物残留量的方法。通过对提取方法和C18固相萃取柱净化条件、色谱条件选择与优化、洗脱液浓度和用量的选择方面的研究,确定采用高效液相色谱分离、荧光检测器检测、外标法定量的分析方法。本方法对环丙沙星、恩诺沙星、氧氟沙星、诺氟沙星、噁喹酸、氟甲喹标准曲线的线性回归系数均在0.99以上,线性范围为0.02～2.0μg/mL。以3倍信噪比RSN计算,环丙沙星、恩诺沙星、诺氟沙星、氧氟沙星检出限为2μg/kg,噁喹酸、氟甲喹检出限为5μg/kg;以10倍信噪比RSN计算,环丙沙星、恩诺沙星、氧氟沙星、诺氟沙星的定量下限为5μg/kg;噁喹酸、氟甲喹的定量下限为10μg/kg。在南美白对虾、罗非鱼、鳗鱼、斑点叉尾鮰中进行这6种喹诺酮类药物加标回收率的验证实验,实验结果满意,回收率在78.8%～92.9%之间;相对标准偏差为2.97%～7.10%。说明本方法简单、灵敏,结果可靠,可用于水产品中环丙沙星、恩诺沙星、氧氟沙星、诺氟沙星、噁喹酸、氟甲喹的同时检测。
译  名：
High Performance Liquid Chromatographic Method for Simultaneous Determination of Six Quinolone Residues in Aquatic Products
作  者：
QIAN Zhuo-zhen1,2,SU Xiu-hua3,WEI Bo-juan4,WU Cheng-ye1,*(1.Fisheries Research Institute of Fujian,Xiamen 361012,China;2.College of Materials,Xiamen University,Xiamen 361005,China;3.College of Food Science,Fujian Agriculture and Forestry University,Fuzhou 350002,China;4.College of Bioengineering,Jimei University,Xiamen 361021,China)
关键词：
reversed-phase high performance liquid chromatography(RP-HPLC);fluorescence spectroscopy;quinolones ;multi-residue determination;aquatic products
摘  要：
A solid-phase extraction followed by reversed-phase high performance liquid chromatographic(SPE-RP-HPLC) method was presented for the simultaneous determination of 6 quinolone residues(enrofloxacin,ciprofloxacin,norfloxacin,ofloxacin,oxolinic acid and flumequine) in aquatic products.Sample extraction,cleanup on a C18 cartilage column and chromatographic separation were investigated.A RP-HPLC system equipped with fluorescence detector(λex = 280 nm,λem = 480 nm) was used for analyzing 6 quinolones,and their quantification was achieved by external standard method.Six quinolones exhibited good linearity within the range of 0.02-2.0 μg/mL and the regression coefficients were all over 0.99.The developed method showed limits of detection of 2 μg/kg for ciprofloxacin,enrofloxacin,norfloxacin,ofloxacin and 5 μg/kg for oxolinic acid and flumequine(RSN = 3),and limits of quantification of 5 μg/kg for ciprofloxacin,enrofloxacin,norfloxacin,ofloxacin and 10μg/kg for oxolinic acid and flumequine(RSN = 10).Satisfying results were obtained in spike recovery experiments and average spike recoveries of 5 replicates at three levels were within the range of 78.8%-92.9%,with RSD range of 2.97%-7.10%.This method,thanks to its simplicity,sensitivity and reliability,has good suitability for the simultaneous determination of 6 quinolone residues in aquatic products.

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