In this study, the strategy of unique adsorbent combined with isotope labeled internal standards was used to significantly reduce the matrix effect for the enrichment and analysis of nine fluoroquinolones in a complex sample by liquid chromatography coupled to quadrupole linear ion trap mass spectrometry (LC-QqQ_LIT-MS/MS). The adsorbent was prepared conveniently by functionalizing Fe₃O₄@SiO₂ microspheres with phenyl and tetrazolyl groups, which could adsorb fluoroquinolones selectively via hydrophobic, electrostatic, and π–π interactions. The established magnetic solid-phase extraction (MSPE) method as well as using stable isotope labeled internal standards in the next MS/MS detection was able to reduce the matrix effect significantly. In the process of LC-QqQ_LIT-MS/MS analysis, the precursor and product ions of the analytes were monitored quantitatively and qualitatively on a QTrap system equipped simultaneously with the multiple reaction monitoring (MRM) and enhanced product ion (EPI) scan. Subsequently, the enrichment method combined with LC-QqQ_LIT-MS/MS demonstrated good analytical features in terms of linearity (7.5–100.0 ng mL^-1, r > 0.9960), satisfactory recoveries (88.6%–118.3%) with RSDs < 12.0%, LODs = 0.5 μg kg^-1 and LOQs = 1.5 μg kg^-1 for all tested analytes. Finally, the developed MSPE-LC-QqQ_LIT-MS/MS method had been successfully applied to real pork samples for food-safety risk monitoring in Ningxia Province, China.

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