Development and validation of an ion pairing LC-Q-Orbitrap method with diverter valve for the quantitative analysis of aminoglycosides in animal-derived matrices and honey for routine applications.

A robust and comprehensive analytical method was developed and validated for the simultaneous identification and quantification of aminoglycosides (AGs) in animal-derived food products and honey. The method employed extraction with 5 % TCA and 0.22 M Na₂EDTA, followed by SPE using HLB cartridges and analysis by LC-Q-Orbitrap HRMS with a diverter valve to protect MS from ion pairing suppression effects. Validation was performed in accordance with CIR EU 2021/808 at three concentration levels from 20 to 7500 μg/kg, yielding mean recoveries of 67.1 %-132.7 %, except for spectinomycin in liver, which ranged from 49.4 % to 61.3 %. LOD and LOQ ranged from 0.01 to 7.0 μg/kg and 0.03 to 22.4 μg/kg, respectively, while CCα and CCβ ranges were 27.3 to 2360.1 μg/kg and 25.2 to 1069.3 μg/kg, respectively. Analysis of 100 samples from Egyptian local markets, including 25 samples each of liver, meat, milk, and honey, revealed AG residues in 80 % of honey samples, while none were detected in the other matrices. The method's applicability was confirmed through successful participation in proficiency testing (PT).