Abstract

A simple, rapid and sensitive screening method by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the identification of 7 macrolides (clarithromycin, erythromycin, oleandomycin, spiramycin, tilmicosin, troleandomycin and tylosin) and 8 quinolones (ciprofloxacin, difloxacin, enrofloxacin, flumequine, moxifloxacin, nalidixic acid, norfloxacin and ofloxacin) in meat and egg-based baby foods. Sample preparation was performed using an alkaline modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) extraction method without additional clean-up steps. A simplex-lattice mixture experimental design was used in the optimization of the QuEChERS extraction solvent. The developed method was successfully validated according to the Commission Decision 2002/657/EC and the European Community Reference Laboratories Residues Guidelines regarding the validation of screening methods 20/01/2010, adopting a fixed permited tolerance for relative ion ratio. Samples of baby food (n = 44) commercialized in Rio de Janeiro, Brazil, were analyzed using the validated method and none of them presented residues of the searched macrolides and quinolones, with a screening target value of 5 µg kg⁻¹.

抽象的

建立了一种简单，快速，灵敏的液相色谱-串联质谱（LC-MS / MS）筛选方法，用于鉴定7种大环内酯类（克拉霉素，红霉素，油橄榄霉素，螺旋霉素，替米考星，曲安霉素和泰乐菌素）和8种喹诺酮类药物（环丙沙星） ，肉类和鸡蛋类婴儿食品中的，地氟沙星，恩诺沙星，氟美卡因，莫西沙星，萘啶酸，诺氟沙星和氧氟沙星）。使用碱性修饰的QuEChERS（快速，简便，廉价，有效，坚固，安全）提取方法进行样品制备，而无需其他清理步骤。在QuEChERS萃取溶剂的优化中使用了单纯形-晶格混合物实验设计。根据委员会决定2002/657 / EC和欧洲共同体参考实验室残留物准则，关于筛选方法的验证已成功验证了所开发的方法，采用相对离子比率的固定允许公差，方法为20/01/2010。使用经过验证的方法对在巴西里约热内卢商业化的婴儿食品样本（n = 44）进行了分析，没有一个样本显示出所搜索的大环内酯类和喹诺酮类药物的残留，筛查目标值为5 µg kg^-1。