高效液相色谱法检测海水养殖环境中喹诺酮类药物残留

Determination of quinolones drug residues in aquacultural seawater using HPLC method

建立了一种养殖海水中诺氟沙星、环丙沙星和恩诺沙星3种喹诺酮类抗生素残留量的高效液相色谱-荧光测定方法。水样经稀盐酸调pH后经HLB固相萃取柱富集、净化,用外标法定量。结果表明,诺氟沙星、环丙沙星和恩诺沙星检出限分别是2、1和1μg/L,定量限分别是6.6、3.3和3.3μg/L,添加浓度为10、20和50μg/L时,3种物质的回收率为71.9%～85.3%,批内变异系数≤10%,批间变异系数≤7%。利用该方法对黄海沿岸部分养殖场及近岸海水(北起36°40.303′N,121°8.939′E;南至35°39.36′N,119°52.433′E)进行分析,诺氟沙星、环丙沙星、恩诺沙星的检出质量浓度分别为6.20～982、55.2和11.6～55.4μg/L。实验结果表明,该方法灵敏度高,重现性好,适用于养殖海水中诺氟沙星、环丙沙星和恩诺沙星的检测。

A detection method of high-performance liquid chromatography （HPLC） coupled with fluorescence was developed for the determination of residues of three quinolones in seawater, pH of were water samples adjusted with dilute HCl followed by extraction and concentration through hydrophilic-lipophilic balance cartridges, and three antibiotic quinolone compounds were determined using external standard quantification method. The results showed that the detection limits of norfloxacin, eiprofloxacin and enrofloxacin were 2 μg/L, 1 μ/L and 1 μg/L respectively, and the quantitative limits were 6.6μg/L, 3.3μg/L and 3.3 μg/L respectively. The recoveries from natural seawater ranged from 71.9% to 85.3% when the three antibiotics were added at the concentration of 10μg/L, 20μg/L and 50 μg/L for norfloxacin, ciprofloxaein and enrofloxacin, respectively. The coefficients of variation within batches were equal or less than 10%, while that among batches were equal or less than 7%. The method has been successfully applied to the monitoring of the residues in the sea water samples from the Yellow Sea near Qingdao （from 36°40. 303′N,121°8. 939′ E to 35°39.36′N,119°52. 433′ E）. Norfloxacin, ciprofloxacin and enrofloxacin were detected at mass concentrations of 6.20-982 μg/L, 55.2 μg/L and 11.6-55.4μg/L respectively. The results showed that this method posessed high sensitivity and good reproducibility, and can be used for the detection of norfloxacin, ciprofloxacin and enrofloxacin in aquacultural seawater.