Fundamental and Applied Analytical Chemistry Laboratory (LAQAFA), Department of Analytical Chemistry, Chemistry Institute, Fluminense Federal University (UFF), Outeiro de São João Batista, s/n, 24020-141, Valonguinho, Centro, Niterói, RJ, Brazil; Graduate Program in Chemistry, Institute of Chemistry, Fluminense Federal University, Outeiro de São João Batista, s/n, 24020-141, Valonguinho, Centro, Niterói, RJ, Brazil.
Fundamental and Applied Analytical Chemistry Laboratory (LAQAFA), Department of Analytical Chemistry, Chemistry Institute, Fluminense Federal University (UFF), Outeiro de São João Batista, s/n, 24020-141, Valonguinho, Centro, Niterói, RJ, Brazil.
Food Chem. 2019 Jan 30;272:148-156. doi: 10.1016/j.foodchem.2018.08.027. Epub 2018 Aug 14.
A highly sensitive analytical method was developed and validated, following international guidelines, for the determination of the residues of five macrocyclic lactones (MLs) (abamectin, doramectin, eprinomectin, ivermectin and moxidectin) in cheese. The extracts were concentrated by rotary-evaporation and derivatized; no clean-up was necessary. Despite matrix complexity, no significant matrix-effect was verified, and standards were prepared in solvents. Linear working ranges varied from 0.25 to 5.0 μg L. Excellent limits of quantification (0.58-0.87 μg kg), mean recoveries (91-103%), and repeatability and intermediate precision (<5.8%) were obtained. Twenty-two samples of bovine and non-bovine cheeses were analyzed. Twenty-one samples showed residues of at least one ML (between 0.59 and 15.3 μg kg), but moxidectin was never detected; a sample of mozzarella was free of MLs. To the best of our knowledge, this is the first method describing the simultaneous evaluation of these MLs in cheese using HPLC and fluorescence detection.
本研究遵循国际准则，开发并验证了一种高灵敏度的分析方法，用于测定奶酪中五种大环内酯类（ML）（阿维菌素、多拉菌素、埃普里诺菌素、伊维菌素和莫昔克丁）残留量。提取物通过旋转蒸发浓缩并衍生化；无需净化。尽管基质复杂，但未检测到明显的基质效应，且标准品在溶剂中制备。线性工作范围为 0.25-5.0μg/L。获得了出色的定量限（0.58-0.87μg/kg）、平均回收率（91-103%）以及重复性和中间精密度（<5.8%）。分析了 22 个牛和非牛奶酪样品。21 个样品显示至少有一种 ML 残留（0.59 至 15.3μg/kg 之间），但从未检测到莫昔克丁；一种马苏里拉奶酪样品中不含 ML。据我们所知，这是首次使用 HPLC 和荧光检测描述同时评估这些 ML 在奶酪中的方法。
