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。
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.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2010年第6期185-189,共5页
Food Science
基金
福建省地方标准渔业计划项目(闽海渔[2008]143号)
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
reversed-phase high performance liquid chromatography（RP-HPLC）
fluorescence spectroscopy
quinolones
multi-residue determination
aquatic products
