Optimisation and validation of liquid-liquid extraction of aminoglycosides from foods of animal origin

This study focused on evaluating and optimising the liquid-liquid extraction (LLE) method for the multi-residue analysis of seven AGs in bovine liver, meat, milk, and kidney in conjunction with liquid chromatography coupled to a quadrupole-Orbitrap high-resolution mass spectrometry (LC-Q-Orbitrap HRMS) for quantification. Of all the hydrophilic interaction liquid chromatography (HILIC) stationary phases tested, the ZIC-HILIC column yielded the best performance. The method was validated according to Commission Implementing Regulation (CIR) EU 2021/808, which encompassed various concentration ranges from 25–7500 µg/kg. The mean recoveries ranged from 79% for liver matrix to 87% for meat matrix, with coefficients of variation (CV) below 18%. The method exhibited excellent linearity, as indicated by correlation coefficients (R2) greater than 0.9903 across all tested matrices. The decision limit (CCα) and detection capability (CCβ) varied from 62 to 5984 µg/kg and 71 to 6471 µg/kg, respectively. The limits of detection (LOD) and quantification (LOQ) were established between 1 and 45 µg/kg, and 2 and 75 µg/kg, respectively. No AG residues were detected in the 120 samples that were collected from different local markets in Egypt using the developed analytical method.