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0.05 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5μg/kg,达氟沙星的定量下限为0.5μg/kg,恩诺沙星的定量下限为2.5μg/kg,沙拉沙星的定量下限为10μg/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92.2%~107.1%,批内相对标准偏差(RSD)为0.6%~5.8%,批间相对标准偏差为1.5%~5.0%。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。
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 0. 05 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 5,5,0. 5,2. 5 and 10 μg/kg,respectively. The average recoveries for 5 fluoroquinolones were in the range of92. 2%-107. 1% 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 0. 6%-5. 8% and 1. 5%-5. 0%,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.
作者
王成真
刘戎
张嘉慧
沈祥广
杜小溪
匡徐
冯可莹
WANG Cheng-zhen;LIU Rong;ZHANG Jia-hui;SHEN Xiang-guang;DU Xiao-xi;KUANG Xu;FENG Ke-ying(College of Veterinary Medicine,South China Agricultural University,Guangzhou 510642,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2018年第5期615-620,共6页
Journal of Instrumental Analysis
基金
广东省公益性研究与能力建设项目(2015A020209130)