Department of Food Science, School of Food Engineering, University of Campinas (UNICAMP), Rua Monteiro Lobato, 80, CEP 13083-862 Campinas, SP, Brazil.
Agilent Technologies Brasil, Alameda Araguaia 1142, Alphaville, CEP 06455-000 Barueri, SP, Brazil.
Food Res Int. 2021 Feb;140:109865. doi: 10.1016/j.foodres.2020.109865. Epub 2020 Nov 3.
This study was carried out to assess the occurrence of antimicrobial residues in samples of tilapia (Oreochromis niloticus) fillets collected at the State of São Paulo retail market and produced from fish farmed in Brazil. For this purpose, a liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) method was validated and used to quantify residues of 25 antibacterial drugs (2 β-lactams, 8 quinolones, 2 macrolides, 5 sulfonamides, 4 tetracyclines, 3 amphenicols and 1 sulfonamide potentiator). For the sample preparation step the QuEChERS approach was performed. Chromatographic separation was conducted using a Zorbax SB C18 column. Method validation was performed based on European and Brazilian guidelines. The validation parameters (linearity, intra- and inter-day precision, accuracy, decision limit, detection capability and robustness) attended the adopted validation guidelines. Limits of detection and quantitation were also determined. Antimicrobial drug residues were quantitated in the incurred samples by using matrix-matched analytical curves. Oxytetracycline, florfenicol and, for the first time, enrofloxacin residues are reported in tilapia fillet samples from Brazil, though, in accordance with the European and Brazilian regulatory framework. Thus, our results draw attention to the use of veterinary products in fish farming in Brazil. Monitoring of veterinary drug residues is essential to ensure the safety of fish products available to the consumer, as well as to keep fish as a food commodity.
本研究旨在评估巴西养殖罗非鱼鱼片在圣保罗州零售市场采集样本中抗菌药物残留的发生情况。为此，我们建立了一种液相色谱-串联质谱（LC-MS/MS）方法，并对其进行了验证，用于定量分析 25 种抗菌药物（2 种β-内酰胺类、8 种喹诺酮类、2 种大环内酯类、5 种磺胺类、4 种四环素类、3 种酰胺醇类和 1 种磺胺增效剂）的残留。在样品制备步骤中，我们采用了 QuEChERS 方法。采用 Zorbax SB C18 柱进行色谱分离。方法验证基于欧洲和巴西的指导原则进行。验证参数（线性、日内和日间精密度、准确度、决策限、检测限和稳健性）符合采用的验证指南。同时还确定了检测限和定量限。通过使用基质匹配的分析曲线，在实际样品中定量了抗菌药物残留。本研究首次报道了巴西罗非鱼鱼片样品中存在土霉素、氟苯尼考和恩诺沙星残留，这与欧洲和巴西的监管框架一致。因此，我们的研究结果表明，巴西在水产养殖中使用了兽药。监测兽药残留对于确保消费者可获得的鱼类产品的安全性以及保持鱼类作为食品的重要性至关重要。
