Jank Louise, Martins Magda Targa, Arsand Juliana Bazzan, Ferrão Marco Flôres, Hoff Rodrigo Barcellos, Barreto Fabiano, Pizzolato Tânia Mara
a Residue Analysis Laboratory , Laboratório Nacional Agropecuário - LANAGRO/RS , Porto Alegre , Brazil.
b Programa de Pós-Graduação em Química - PPGQ , Universidade Federal do Rio Grande do Sul - UFRGS , Porto Alegre , Brazil.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2018 Oct;35(10):1975-1989. doi: 10.1080/19440049.2018.1508895. Epub 2018 Aug 24.
An increasing concern about food safety has been observed over the years. The presence of drugs residues in food is one of the major subjects of research in food safety. Feedingstuffs can be responsible for carryover into the food chain of residues of several drugs. This paper describes the development, validation and application of a fast and simple method for analysis of 24 antibiotic residues in feedingstuffs for cattle, pigs and poultry. Analytes include compounds from different antimicrobials classes, such as sulfonamides (sulfadiazine, sulfamethazine, sulfamethoxazole, sulfaquinoxaline, sulfachlorpyridazine, sulfadoxine, sulfadimethoxine, sulfizoxazole, sulfamerazine and sulfathiazole), fluoroquinolones (ciprofloxacin, enrofloxacin, norfloxacin, danofloxacin, difloxacin, sarafloxacin, flumequine, nalidixic acid and oxolinic acid), tetracyclines (tetracycline, doxycycline, oxytetracycline and chlortetracycline) and trimethoprim. Samples were extracted with methanol:water (70:30) 0.1% formic acid, followed by clean-up steps using centrifugation, low-temperature purification (LTP) and ultracentrifugation. Instrumental analysis was performed using liquid chromatography coupled to tandem mass spectrometry. Chromatographic separation was achieved using a C18 column and a mobile phase composed of acetonitrile and water, both with 0.1% formic acid. Validation parameters such as limit of detection (LOD), limit of quantification (LOQ), selectivity, linearity, accuracy, precision, decision limit (CCα) and detection capability (CCβ) were determined and meet the adopted criteria. LOD and LOQ were set to 30 and 75 µg kg, respectively. Inter-day precision were in the range from 4.0 to 11.1%, and linearity provides values of r above 0.95 for all analytes. The optimised method was applied to the analysis of more than 1500 real samples within the period 2012-2017. Non-compliant results were discussed and classified in terms of analytes, feed types and target species. Multivariate analysis of the data was performed using principal component analysis.
多年来，人们对食品安全的关注日益增加。食品中药物残留的存在是食品安全研究的主要课题之一。饲料可能会导致多种药物残留进入食物链。本文描述了一种快速简便的方法用于分析牛、猪和家禽饲料中24种抗生素残留的方法的开发、验证及应用。分析物包括来自不同抗菌类别的化合物，如磺胺类（磺胺嘧啶、磺胺二甲嘧啶、磺胺甲恶唑、磺胺喹恶啉、磺胺氯哒嗪、磺胺多辛、磺胺二甲氧嘧啶、磺胺异恶唑、磺胺间甲氧嘧啶和磺胺噻唑）、氟喹诺酮类（环丙沙星、恩诺沙星、诺氟沙星、达氟沙星、二氟沙星、沙拉沙星、氟甲喹、萘啶酸和恶喹酸）、四环素类（四环素、多西环素、土霉素和金霉素）以及甲氧苄啶。样品用甲醇:水（70:30）0.1%甲酸进行提取，随后通过离心、低温净化（LTP）和超速离心进行净化步骤。采用液相色谱 - 串联质谱进行仪器分析。使用C18柱和由乙腈和水组成的流动相（均含有0.1%甲酸）实现色谱分离。测定了检测限（LOD）、定量限（LOQ）、选择性、线性、准确度、精密度、决策限（CCα）和检测能力（CCβ）等验证参数，且均符合采用的标准。LOD和LOQ分别设定为30和75 μg/kg。日间精密度在4.0%至11.1%范围内，所有分析物的线性度r值均高于0.95。该优化方法在2012 - 2017年期间应用于15００多个实际样品的分析。对不符合标准的结果根据分析物、饲料类型和目标物种进行了讨论和分类。使用主成分分析对数据进行了多变量分析。
