| 高效液相色谱法快速测定鸡蛋中5种氟喹诺酮类药物残留 |
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| 基金项目:广东省公益性研究与能力建设项目(2015A020209130) |
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| 中文摘要:建立了一种检测鸡蛋中环丙沙星、达氟沙星、恩诺沙星、二氟沙星及沙拉沙星残留的高效液相色谱方法。该方法前处理简便快速，样品经低浓度乙腈结合加热促使蛋白质快速沉淀，正己烷脱脂，分离清液后进高效液相色谱仪分析。流动相为005 mol/L磷酸/三乙胺溶液-乙腈溶液(80∶20)，荧光检测器的激发波长为280 nm，发射波长为450 nm。该方法对环丙沙星和二氟沙星的定量下限为5 μg/kg，达氟沙星的定量下限为05 μg/kg，恩诺沙星的定量下限为25 μg/kg，沙拉沙星的定量下限为10 μg/kg。在定量下限及低、中、高4种加标浓度下，5种氟喹诺酮类药物的平均回收率为922%~1071%，批内相对标准偏差(RSD)为06%~58%，批间相对标准偏差为15%~50%。方法具有前处理简单、环保、快捷、准确度和灵敏度高等优点，适合生产线和流通环节鸡蛋样品的快速检测。 |
| 中文关键词:高效液相色谱法 氟喹诺酮类药物 药物残留 鸡蛋 快速检测 |
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| Rapid Determination of Five Fluoroquinolones in Eggs by High Performance Liquid Chromatography |
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| Abstract:A high performance liquid chromatography(HPLC) method combined with a rapid and simple pretreatment approach was established for the determination of five fluoroquinolones(ciprofloxacin,danofloxacin,enrofloxacin,difloxacinand and sarafloxacin) residues in eggs.Samples were extracted with acetonitrile.Protein in egg samples was precipitated by heating in water-bath.The supernatants were degreased with n hexane,and followed by HPLC analysis.The mobile phase consisted of 005 mol/L phosphoric acid and triethylamine-acetonitrile(80∶20).The fluorometric excitation wavelength was 280 nm,and the emission wavelength was 450 nm.The limits of quantitation(LOQ) for ciprofloxacin,difloxacin,danofloxacin,enrofloxacin and sarafloxacin were 5,5,05,25 and 10 μg/kg,respectively.The average recoveries for 5 fluoroquinolones were in the range of 922%-1071% at four spiked levels(LOQ,2 LOQ,4 LOQ and 20 LOQ),and the intra day and inter day relative standard deviations(RSDs) were in the ranges of 06%-58% and 15%-50%,respectively.The proposed method is rapid,accurate,sensitive and eco friendly,and could be used for the quick analysis on residues of fluoroquinolones in egg in its production and distribution for consumption. |
| Key Words:HPLC fluoroquinolones residue egg rapid determination |
| 引用本文：王成真，刘戎，张嘉慧，沈祥广,杜小溪，匡徐，冯可莹.高效液相色谱法快速测定鸡蛋中5种氟喹诺酮类药物残留[J].分析测试学报,2018,37(5):615-620. |
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