高效液相色谱法检测多种动物组织中氟喹诺酮类药物残留量的研究

Determination of Fluoroquinolones in Tissues of Several Animals by HPLC

关键词:  氟喹诺酮类药物  残留  动物组织  高效液相色谱法

Key words:  fluoroquinolone  residues  animal tissue  HPLC

摘要:

建立了猪、牛、羊、鸡、兔的肌肉、脂肪、肝脏和肾脏四种组织中环丙沙星、达氟沙星、恩诺沙星、沙拉沙星和二氟沙星残留量检测的高效液相色谱法。试样经磷酸盐溶液提取、经C18固相萃取柱浓缩净化后，用高效液相色谱分析，荧光检测器检测，外标法定量。5种药物在0.1-100 μg/L浓度范围内线性关系良好。环丙沙星、恩诺沙星、沙拉沙星和二氟沙星在五种动物肌肉、脂肪组织中的定量限为5 μg/kg，在肝脏、肾脏组织中的定量限为10 μg/kg；达氟沙星在肌肉、脂肪组织中的定量限为1 μg/kg，在肝脏、肾脏组织中的定量限为2 μg/kg。在指定的三个浓度添加水平下，5种药物在各组织中的平均回收率为62%-103%；批内变异系数为0.30%-18 %，批间变异系数为1.0%-17%。该方法操作简单，准确度和精密度好，动物品种及动物组织覆盖范围广，可以很好地满足实际检测工作的需要。

Abstract:

An HPLC method for the determination of ciprofloxacin,danofloxacin,enrofloxacin, sarafloxacin and difloxacin in muscle, fat, liver and kidney of swine, chicken, cattle, sheep and rabbit been developed. The analytes were extracted with phosphate solution and the supernatant of the extract was applied onto a C18 solid phase extraction column for clean-up. The separation was achieved by HPLC, and the detection was performed with a fluorescence detector. The calibration curves showed nearly perfect linearity between the peak areas and concentrations of fluoroquinolones in range from 0.1 to 100 μg/L. The limit of quantification(LOQ) was 5 μg/kg for ciprofloxacin, enrofloxacin, sarafloxacin and difloxacin in muscle and fat and 10 μg/kg in liver and kidney. As for danofloxacin, the LOQ was 1 μg/kg in muscle and fat and 2 μg/kg in liver and kidney. The average recoveries at the three assigned concentrations were 62%-103%, intra - and inter - batch variation coefficients were 0.30%-18% and 1.0%-17%. This simple, fast HPLC method with high accuracy and precision can be applied in detection of FQs in diverse animal tissues from various animal species, which is considered sufficient for routine analysis.