Determination of quinolones and fluoroquinolones, tetracyclines and sulfonamides in bovine, swine and poultry liver using LC-MS/MS

作者：Martins Magda Targa^*; Barreto Fabiano; Hoff Rodrigo Barcelos; Jank Louise; Arsand Juliana Bazzan; Feijo Tiago Correa; Scherman Schapoval Elfrides Eva

来源：Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure& Risk Assessment, 2015, 32(3): 333-341.

DOI：10.1080/19440049.2015.1007091

• food control
• validation
• bovine liver
• mass spectrometry
• antibacterials

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 2.0xthe 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 (CC alpha) and detection capability (CC beta), were also evaluated.

• 出版日期2015-3-4