Martins Magda Targa, Barreto Fabiano, Hoff Rodrigo Barcelos, Jank Louise, Arsand Juliana Bazzan, Feijó Tiago Correa, Schapoval Elfrides Eva Scherman
a Ministério da Agricultura , Pecuária e Abastecimento, Laboratório Nacional Agropecuário - LANAGRO/RS , Porto Alegre , RS , Brazil.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2015;32(3):333-41. doi: 10.1080/19440049.2015.1007091. Epub 2015 Feb 16.
Antibacterials are widely used in veterinary medicine. Residues of these drugs can remain in food of animal origin, including bovine liver. This paper describes a fast and simple analytical method for the determination of quinolones and fluoroquinolones, tetracyclines and sulfonamides in bovine liver samples. Deuterated enrofloxacin, sulfapyridine and demeclocycline were used as internal standards. The homogenised liver samples were extracted with acidified acetonitrile. Steps of non-solid-phase extraction (SPE) clean-up and concentration were used in the presented method. The final extracts were analysed by sensitive and selective detection of all components in a single run using LC-MS/MS. Acceptable recoveries between 66% and 110% were obtained. Good linearity (r(2)) above 0.96, considering three different days, for all drugs was achieved in concentrations ranging from 0.0 to 2.0 × the maximum residue limit (MRL). Intraday precision with coefficient of variation (CV%) (n = 6) lower than 14.7% and inter-day precision lower than 18.8% in agreement with European Commission Decision 2002/657/EC were obtained in concentrations ranging from 0.5 to 1.5 MRL. Accuracy was between 86% and 110%. Limits of detection and quantitation, as well as decision limit (CCα) and detection capability (CCβ), were also evaluated.
抗菌药物在兽医学中广泛使用。这些药物的残留可存在于包括牛肝在内的动物源性食品中。本文描述了一种快速简便的分析方法，用于测定牛肝样品中的喹诺酮类、氟喹诺酮类、四环素类和磺胺类药物。氘代恩诺沙星、磺胺吡啶和地美环素用作内标。将匀浆后的肝脏样品用酸化乙腈萃取。本方法采用非固相萃取（SPE）净化和浓缩步骤。最终提取物通过液相色谱-串联质谱（LC-MS/MS）在一次进样中对所有成分进行灵敏且选择性的检测进行分析。回收率在66%至110%之间，可接受。在浓度范围为0.0至2.0倍最大残留限量（MRL）时，考虑三天的数据，所有药物的线性关系良好（r(2)），均高于0.96。在浓度范围为0.5至1.5 MRL时，日内精密度变异系数（CV%）（n = 6）低于14.7%，日间精密度低于18.8%，符合欧盟委员会第2002/657/EC号决定。准确度在86%至110%之间。还评估了检测限、定量限以及决策限（CCα）和检测能力（CCβ）。
