牛奶中氟喹诺酮类药物残留量检测方法研究

Study on deterction Method of fluroquinolones residues in milk

关键词:  高效液相色谱法  氟喹诺酮类药物  残留  牛奶

Key words:  HPLC  fluroquinolones drug  residues  milk

摘要:

建立了牛奶中五种氟喹诺酮类药物（达氟沙星、恩诺沙星、环丙沙星、沙拉沙星和二氟沙星）残留检测的高效液相色谱-荧光检测法。实验结果表明，环丙沙星、恩诺沙星、沙拉沙星、二氟沙星在0.005-0.3µg/mL，达氟沙星在0.001-0.06µg/mL浓度范围内，呈良好的线性关系，相关系数均大于0.999。方法最低检测限环丙沙星、恩诺沙星、沙拉沙星、二氟沙星为5ng/mL，最低定量限为10 ng/mL。达氟沙星最低检测限为1 ng/mL，最低定量限为2 ng/mL。环丙沙星、恩诺沙星、沙拉沙星、二氟沙星在10、50、100 ng/mL三种浓度添加水平上，平均回收率在70-94%，达氟沙星在2、10、20 ng/mL三种浓度添加水平上，平均回收率在73-88%。批内、批间变异系数均小于11%。

Abstract:

A method for determination of five fluroquinolones drug residues (danofloxacin. enrofloxacin. Ciprofloxacin. Sarafloxacin. difloxacin) in milk with HPLC by fluorescence detection was established. The calibration curve was good liner between the ratio of the peak areas and concentrations of ciprofloxacin. enrofloxacin. sarfloxacin. difloxacin. sarafloxacin from 0.005-0.5µg/mL and of danofloxacin from 0.001-0.1µg/mL .The correlation coefficiont were all more than 0.9999.The detection limit of the method of danofloxacin was 1 ng/mL and the others wrer 5ng/mL.The limit of quantification of danofloxacin was 2 ng/mL and the others were 10ng/mL.The average recoveries of danofloxacin from spiked milk at the three concentrations of 2、10、20ng/mL ranged from 73-88% and the others at the three concentrations of 10、50、100ng/mL ranged from 70-94%. In day-between days batch coefficients of variation were both less than 11%.