Liang Feiyan, Liu Huawen, Li Minglu, Zhang Ronglin, Xin Lina, Yang Huijing, Zhang Yun
Guangxi-Asean Food Inspection and Testing Center, Food Safety Monitoring and Evaluation Center, Nanning, China.
Technology Innovation Center of Natural Fragrances and Flavors, State Administration for Market Regulation, Guangxi, China.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2025 Sep;42(9):1192-1212. doi: 10.1080/19440049.2025.2537865. Epub 2025 Aug 1.
Aminoglycosides (AGs) are broad-spectrum bactericidal antibiotics commonly used in animal husbandry. Residues of AGs in food can enter the human body through the food chain and biomagnification. Due to the specific structure and properties of AGs, it is difficult to achieve adequate extraction and separation during analysis, often giving rise to matrix effects. An LC-MS/MS analysis after cleanup based on dipole interaction, hydrogen bonding, adsorption and ion interaction, was developed to determine 16 AGs residues in livestock and poultry meat. The samples were extracted with phosphate buffer (pH 4.0, containing trichloroacetic acid, EDTA-2Na, 0.05 moL L sodium pentanesulfonate, and sodium hexanesulfonate), purified by HLB solid-phase extraction column, and retained and separated by HILIC column with hydrophilic interaction. High correlation coefficients ( > 0.99) of calibration curves for the analytes were obtained, linear from 25 to 1500 ng mL. The detection limits were 0.006-1.0 μg kg, the limits of quantification were 0.02-3.0 μg kg. Reasonable recoveries (61%-119%) were demonstrated with acceptable relative standard deviation (RSD < 18%) at 50, 250, and 500 μg kg. The signals due to most AGs were affected by different strong matrix effects of livestock and poultry meat, and showed different inhibition and enhancement phenomena, resulting in false negative/positive misjudgments in the results. In terms of overall data and consideration, this method should be an efficient approach for multi-residue analysis as a reliable, selective, and highly sensitive methodology for the simultaneous quantification and confirmation of AGs in livestock and poultry meat.