【摘要】 基于氟喹诺酮类药物与铽离子形成配合物后的荧光增强作用,建立了同时检测鸡肉中氟喹诺酮类(FQs)药物环丙沙星、诺氟沙星和恩诺沙星残留的Tb3+增敏高效液相色谱(HPLC)柱后衍生荧光检测方法。优化的实验条件如下:流动相为0.05mol/L醋酸/醋酸钠缓冲液(pH6.0)-乙腈(体积比为89∶11),色谱柱为Hypersil BDS-C18,柱温40℃,流速0.8mL/min;Tb3+浓度为8×10-5mol/L;衍生反应温度40℃,衍生泵流速0.5mL/min;荧光检测激发波长271nm,发射波长545nm。实验结果表明,将上述3种药物以1.0,10.0,50.0,100.0ng/g水平添加到鸡肉后的回收率范围为66.3%~88.0%,相对标准偏差(RSD)均小于15.0%。定量分析的线性范围为0.1~500ng/mL,方法的日内和日间RSD均小于13.0%;最低检出限分别为0.05(环丙沙星)、0.05(诺氟沙星)和0.08(恩诺沙星)ng/g,比前人报道的非衍生高效液相色谱荧光检测法检测FQs药物的灵敏度有极大的提高。该项研究为FQs药物多残留检测提供了灵敏度更高的新方法。更多还原

【Abstract】 A method of high performance liquid chromatography with post-column derivatization and terbium sensitized fluorescence for simultaneous determination of residues of ciprofloxacin,norfloxacin and enrofloxacin in chicken was established,based on the effect that Tb3+ can sensibilize fluorescence of fluoroquinolones.Under the optimal chromatographic condition,three fluoroquinolones were separated on a C18 column with 0.05 mol/L acetic acid/acetate buffer-acetonitrile(89∶11,v/v) as the mobile phase,and at a flow rate of 0.8 mL/min;then were derivatized with 8×10-5 mol/L Tb3+ at 40 ℃,and at a flow rate of 0.5 mL/min;finally were detected using a fluorescence detector(λex=271 nm,λem=545 nm).The recoveries of three fluoroquinolones ranged from 66.3%-88.0% at the added levels of 1.0,10.0,50.0,and 100.0 ng/g,and the relative standard deviations(RSDs) were less than 15.0%.The linear range for quantitative analysis was between 0.1 and 500 ng/mL.All the RSDs of the inter-day and intra-day analyses were less than 13.0%.The detection limits were 0.05 ng/g for ciprofloxacin and norfloxacin and 0.08 ng/g for enrofloxacin.The method is sensitive for the determination of multi-residues of fluoroquinolones in chicken.更多还原