Qi Kezong, Zhu Liangqiang, Sun Guoren, Shi Zuhao, Peng Kaisong
College of Animal Science and Technology, Anhui Agricultural University, Hefei 230036, China.
Se Pu. 2007 Jul;25(4):553-6.
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 x 10(-5) mol/L Tb3+ at 40 degrees C, and at a flow rate of 0.5 mL/min; finally were detected using a fluorescence detector (lamda(ex) = 271 nm, lamda(em) = 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.
基于Tb3+能敏化氟喹诺酮类药物荧光的效应,建立了一种柱后衍生化-铽敏化荧光高效液相色谱法,用于同时测定鸡肉中恩诺沙星、环丙沙星和诺氟沙星的残留量。在最佳色谱条件下,采用C18柱,以0.05 mol/L乙酸/乙酸盐缓冲液-乙腈(89:11,v/v)为流动相,流速为0.8 mL/min,分离三种氟喹诺酮类药物;然后在40℃下用8×10(-5) mol/L Tb3+进行衍生化,流速为0.5 mL/min;最后用荧光检测器检测(激发波长λ(ex)=271 nm,发射波长λ(em)=545 nm)。三种氟喹诺酮类药物在1.0、10.0、50.0和100.0 ng/g添加水平下的回收率为66.3%-88.0%,相对标准偏差(RSD)小于15.0%。定量分析的线性范围为0.1至500 ng/mL。日内和日间分析的所有RSD均小于13.0%。环丙沙星和诺氟沙星的检出限为0.05 ng/g,恩诺沙星的检出限为0.08 ng/g。该方法对鸡肉中氟喹诺酮类药物多残留的测定具有较高的灵敏度。