Freitas Andreia, Barbosa Jorge, Ramos Fernando
INIAV-LNIV, Laboratório Nacional de Investigação Veterinária, Estrada de Benfica, 701, 1549-011 Lisboa, Portugal.
CNC - Centro de Neurociências e Biologia Celular, Pólo das Ciências da Saúde, Faculdade de Farmácia, Universidade de Coimbra, Azinhaga de Santa Comba, 3000-548 Coimbra, Portugal.
Meat Sci. 2014 Sep;98(1):58-64. doi: 10.1016/j.meatsci.2014.04.003. Epub 2014 Apr 18.
A multi-residue quantitative screening method covering 41 antibiotics from 7 different families, by ultra-high-performance-liquid-chromatography tandem mass spectrometry (UHPLC-MS/MS), is described. Sulfonamides, trimethoprim, tetracyclines, macrolides, quinolones, penicillins and chloramphenicol are simultaneously detected after a simple sample preparation of bovine muscle optimized to achieve the best recovery for all compounds. A simple sample treatment was developed consisting in an extraction with a mixture of acetonitrile and ethylenediaminetetraacetic acid (EDTA), followed by a defatting step with n-hexane. The methodology was validated, in accordance with Decision 2002/657/EC by evaluating the required parameters: decision limit (CCα), detection capability (CCβ), specificity, repeatability and reproducibility. Precision in terms of relative standard deviation was under 20% for all compounds and the recoveries between 91% and 119%. CCα and CCβ were determined according the maximum residue limit (MRL) or the minimum required performance limit (MRPL), when required.
本文描述了一种采用超高效液相色谱串联质谱法(UHPLC-MS/MS)对来自7个不同家族的41种抗生素进行多残留定量筛查的方法。在对牛肌肉样本进行简单预处理以实现所有化合物的最佳回收率后,可同时检测磺胺类药物、甲氧苄啶、四环素、大环内酯类、喹诺酮类、青霉素类和氯霉素。开发了一种简单的样品处理方法,先用乙腈和乙二胺四乙酸(EDTA)混合物进行萃取,然后用正己烷进行脱脂步骤。该方法根据2002/657/EC号决定进行了验证,通过评估所需参数:决策限(CCα)、检测能力(CCβ)、特异性、重复性和再现性。所有化合物的相对标准偏差精度均低于20%,回收率在91%至119%之间。必要时,根据最大残留限量(MRL)或最低所需性能限量(MRPL)确定CCα和CCβ。