Establishment and verification of GC-MS/MS method for four fluoroquinolones residues determination based on precolumn derivatization: Application to poultry eggs

In this study, liquid‒liquid extraction and solid‒phase extraction were coupled with derivatization to detect 4 types of fluoroquinolones residues in poultry eggs (chicken, duck, goose, and quail eggs) via GC-MS/MS. A 10% trichloroacetic acid‒acetonitrile solution and trimethylsilyl diazomethane (TMSD) were chosen as the extraction and derivatization reagents, respectively. The results revealed that the detection and quantitative limits (LODs, LOQs) were 1.0, 0.2, 0.5, and 1.0 μg/kg and 2.0, 0.4, 1.0, and 2.0 μg/kg, respectively. The peak areas of all the target compounds had a good linear relationship with the corresponding concentrations of the matrix matched standard working solution, with R² values higher than 0.9991. The recoveries of the target compounds were all higher than 78.0%. The RSDs ranged from 2.1% to 8.0%. All the matrices had weak matrix effect. This established method satisfied the requirements of the NY/T 1896–2010 industry standard for veterinary drug residue detection in China, providing a scientific basis for fluoroquinolone residue detection. Furthermore, this method expands the monitoring range, improves the detection efficiency, reduces the cost, and meets the detection needs of different laboratories.