| 摘要: |
| 为减少有机试剂使用，减轻环境污染，提高检测效率，建立了可同时检测鸡蛋中氧氟沙星（Ofloxacin，OFL）、培氟沙星（Pefloxacin，PEF）、环丙沙星（Ciprofloxacin，CIP）、达氟沙星（Danofloxacin，DAN）、恩诺沙星（Enrofloxacin，ENR）和沙拉沙星（Sarafloxacin，SAR）6种氟喹诺酮类药物残留的环境友好型高效液相色谱荧光检测方法。鸡蛋样品用纯水提取，氯化钠盐析，加热冷冻净化，正己烷脱脂，采用0.5%甲酸水-乙腈体系作为流动相，荧光激发波长280 nm，发射波长450 nm检测。结果显示：OFL的线性范围为8~1 000 μg/kg，DAN为0.4~50.0 μg/kg，其余4种均为2~250 μg/kg，相关系数大于0.99。OFL检测限为4 μg/kg，DAN为0.2 μg/kg，其余4种均为1 μg/kg；OFL定量限为20 μg/kg，DAN为1μg/kg，其余4种均为5 μg/kg。6种药物添加平均回收率为80.52%~101.10%；相对标准偏差为2.99%~10.40%。 |
| 关键词: 氟喹诺酮类药物 高效液相 鸡蛋 药物残留 环境友好 |
| DOI：10.11841/j.issn.1007-4333.2017.04.12 |
| 投稿时间：2016-04-20 |
| 基金项目:农业部公益性行业（农业）科研专项经费项目（201203069-2） |
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| Development of environment-friendly HPLC method for simultaneous determination of six fluoroquinolones in eggs |
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CHENG Yongxiang, XIA Xi, ZHANG Pengchun, ZHAO Kunxia, LI Xiaowei, DING Shuangyang
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| (College of Veterinary Medicine, China Agricultural University, Beijing 100093, China) |
| Abstract: |
| In order to reduce the use of organic regents,decrease the pollution of environment and increase the efficiency of detection,an analytical method for simultaneous determination of six fluoroquinolones (FQs,including ofloxacin,peflocacin,ciproflocacin,danofloxacin,enrofloxacin and sarafloxacin) residues in eggs based on high performance liquid chromatography with fluorescence detection (HPLC/FLD) was established.Samples were extracted by water and added NaCl to salt out.The extracts were heated and frozen,degreased by n-hexane.Six FQs were separated by C18 column with 0.5% methanoic acid/acetonitrile as the mobile phase and detected with fluorescence detection.The fluorometric excitation wavelength was 280 nm,and emission wavelength was 450 nm.The tested ranges of quinolone calibrations were 0-1 000 μ g/kg for ofloxacin,0-50 μ g/kg for danofloxacin,0-250 μ g/kg for the other four FQs with the correlation coefficients greater than 0.99.The limits of detection (LODs) were ofloxacin 4 μ g/kg,danofloxacin 0.2 μ g/kg,and the other four FQs 1 μ g/kg. And the limits of quantification (LOQs) were ofloxacin 20 μ g/kg, danofloxacin 1 μ g/kg,and the other four FQs 5 μ g/kg.The average percentage recoveries were ranged from 80.52% to 101.10% for six FQs in eggs samples,coefficients of variability (CV) were ranged from 2.99%-10.40%. |
| Key words: fluoroquinolones high performance liquid chromatography egg residue environment-friendly |
