Department of Analytical Chemistry, Institute of Chemistry, University of Campinas, PO Box 6154, 13084-971 Campinas, SP, Brazil.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2009 Oct;26(10):1331-40. doi: 10.1080/02652030902822778.
A method for the simultaneous determination of flumequine, oxolinic acid, sarafloxacin, danofloxacin, enrofloxacin, and ciprofloxacin in tilapia (Orechromis niloticus) fillet, using high-performance liquid chromatography with fluorescence detection (HPLC-FLD) is presented. The quinolones were extracted from the food matrix with a solution of 10% trichloroacetic acid and methanol (80:20 v/v). Clean-up of the extract was performed using polymeric solid-phase extraction cartridges. Identification of the quinolones was confirmed by liquid chromatography-tandem mass spectrometry. The HPLC-FLD method was validated in-house and the following analytical parameters were obtained: linearity higher than 0.99 for all the quinolones; intra- and interassay precisions were lower than 3.5% and 10.9%, respectively; and recoveries ranged from 73% to 110%. The limit of quantification was below the maximum residue limit established by the Joint Expert Committee on Food Additives (JECFA), which indicates that the method is appropriate for the determination of quinolones in fish fillet.
本文建立了一种利用高效液相色谱-荧光检测法（HPLC-FLD）同时检测罗非鱼片（Oreochromis niloticus）中氟甲喹、恶喹酸、沙拉沙星、丹诺沙星、恩诺沙星和环丙沙星的方法。采用 10%三氯乙酸和甲醇（80:20，v/v）溶液从食物基质中提取喹诺酮类药物。采用聚合物固相萃取小柱对提取物进行净化。采用液相色谱-串联质谱法对喹诺酮类药物进行鉴定。该 HPLC-FLD 方法在内部进行了验证，得到了以下分析参数：所有喹诺酮类药物的线性均大于 0.99；日内和日间精密度分别低于 3.5%和 10.9%；回收率在 73%至 110%之间。定量限低于食品添加剂联合专家委员会（JECFA）规定的最大残留限量，表明该方法适用于鱼片中喹诺酮类药物的检测。
