Freitas Andreia, Leston Sara, Rosa João, Castilho Maria da Conceição, Barbosa Jorge, Rema Paulo, Pardal Miguel Ângelo, Ramos Fernando
a INIAV-LNIV, Laboratório Nacional de Investigação Veterinária , Lisbon , Portugal.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2014;31(5):817-26. doi: 10.1080/19440049.2014.891764. Epub 2014 Apr 7.
This paper describes a method for the determination of 41 antibiotics from seven different classes in gilthead sea bream (Sparus aurata) by ultra-high-performance liquid chromatography with tandem mass spectrometry (UPLC-MS/MS). Sulfonamides, trimethoprim, tetracyclines, macrolides, quinolones, penicillins and chloramphenicol were simultaneously determined. Fourteen procedures for sample treatment were tested and an extraction with acetonitrile and ethylenediaminetetra acetic acid was found to be the best option. The methodology was validated in accordance with Decision 2002/657/EC. Precision in terms of relative standard deviation (RSD) was under 17% for all compounds, and the recoveries ranged from 92% to 111%. CCα and CCβ were determined according to the maximum residue limit or the minimum required performance limit, when necessary. The validation provided evidence that the method was suitable for application in routine analysis for the detection and confirmation of antibiotics in muscle of gilthead sea bream, an important and intensively produced fish in aquaculture.
本文描述了一种采用超高效液相色谱-串联质谱法(UPLC-MS/MS)测定金头鲷(Sparus aurata)中7个不同类别的41种抗生素的方法。该方法可同时测定磺胺类、甲氧苄啶、四环素类、大环内酯类、喹诺酮类、青霉素类和氯霉素。测试了14种样品处理程序,发现用乙腈和乙二胺四乙酸萃取是最佳选择。该方法依据2002/657/EC号决定进行了验证。所有化合物的相对标准偏差(RSD)精密度均在17%以下,回收率在92%至111%之间。必要时,根据最大残留限量或最低所需性能限量测定CCα和CCβ。验证结果表明,该方法适用于金头鲷肌肉中抗生素检测和确证的常规分析,金头鲷是水产养殖中一种重要且集约化生产的鱼类。