Simultaneous determination of the four key fluoroquinolones and two antipsychotics in fish and shrimp by LC-MS/MS

In this study, we developed and validated a liquid chromatography triple quadrupole tandem mass spectrometry (LC-MS/MS) method used to simultaneously determine levels of four fluoroquinolones (ofloxacin, norfloxacin, lomefloxacin, and pefloxacin) and two antipsychotics (diazepam and methaqualone) in fish and shrimp. The samples were extracted with a mixture of anhydrous sodium sulfate and acetonitrile, and purified by C₁₈ cartridge solid-phase extraction with an optimized eluent. The MS² method was applied to recognize the molecular structure of these compounds according to a main fragmentation scheme. The key ions of identification and quantification were deduced from chemical structures. Multiple reaction monitoring was used to quantitatively analyse the compounds of interest. Satisfactory linearities were obtained (R² ≥0.99) with the limits of quantitation (LOQs) ranging between 0.03 and 1.96 μg kg^-1. The recoveries were 74-122%, with a relative standard deviation (RSD) below 4.9% for these compounds at the spiking level of three, five, and ten times the LODs, respectively. The LC-MS/MS method allows precise and sensitive determination of residues of six important banned veterinary drugs in fish and shrimp tissue. This methodological approach solved the problem imposed by the need for two or more analysis methods to analyse the compounds of interest described in this study.