高效液相色谱-荧光检测畜禽粪污中四种氟喹诺酮类抗生素残留

为了建立高效液相色谱-荧光测定畜禽粪污中氧氟沙星、诺氟沙星、环丙沙星、恩诺沙星残留的分析方法,将畜禽粪便样品经乙腈超声提取,再经正己烷液-液萃取,并经氮吹浓缩,乙腈与水混合溶解残渣,过微孔滤膜,采用高效液相色谱-荧光检测,以0.01 mol/L四丁基溴化胺(pH 3.0)/乙腈(94/6,V/V)为流动相,于激发波长280 nm、发射波长480 nm处进行检测。结果表明,畜禽粪污样品中4种喹诺酮类抗生素的平均回收率为77.8%～98.2%,相对标准偏差为3.5%～7.2%,检测限为0.005～0.010μg/kg。该方法简便、快速,可满足畜禽粪污中4种喹诺酮类兽药残留量的同时检测。

Determination of Four Kinds of Fluoroquinolones Antibiotics Residues in Livesotck Feces by High Performance Liquid Chromatography-Fluorescence Detection

A reversed-phase high performance liquid chromatography method has been developed for the simultaneous determination of four fluoroquinolones antimicrobial residues in livesotck feces.The samples were ultrasonically extracted by acetonitrile,followed by a double liquid-liquid extraction with n-hexane.After the solvent was vaporized by nitrogen stream,four analytes were analysed by high performance liquid chromatography-fluorimetric detection with excitation and emission wavelength of 280 nm and 480 nm,respectively,using 0.01 mol / L tetrabutyl ammonium bromide(pH 3.0) / acetonitrile(94 / 6,V/V) as the mobile phase.The average recoveries of the four fluoroquinolones in livesotck feces ranged from 77.8% to 98.2%,and relative standard deviation were 3.5%～7.2%.The detective limit for four quinolones were from 0.005 to 0.010 μg / kg.The results indicated that the developed multiresidues method were easy and fast.It has also demonstrated that the method could meet the requirements for simultaneous determination of four kinds of fluoroquinolones antibiotics in livestock feces.