RESUMO
For the simultaneous identification and quantification of five nitrofurans metabolites in farmed shrimp and fish, 3-amino-2-oxazolidinone (AOZ), 3-amino-5-morpholinomethyl-2-oxazolidinone (AMOZ), 1-aminohydantoine (AHD), semicarbazide (SEM), and 3,5-dinitrosalicylic acid hydrazide (DNSH), an accurate, precise, and specific method was developed. The mixture of water and methanol (60/40; v/v) was found to be the final optimised solvent for injection. The analytical run duration was 7 min, and the mobile phase included 2 mM methanol and ammonium formate. The new reference point for action (RPA) of 0.50 µg kg-1 as per EC/1871/2019 was taken into consideration and evaluated for the performance characteristics as per the CIR (EC)/2021/808 criteria. Specificity, relative retention time (≤0.25%) relative ion ratio (≤40%), linearity (0.25 to 2.0 µg kg-1), trueness (between 82.8 and 118.1%), repeatability (RSDr ≤14%), within lab reproducibility (RSDwr ≤16.9%), CCα (0.32-0.36 µg kg-1), ruggedness and relative matrix effect (≤14.26%) achieved acceptable values.
Assuntos
Nitrofuranos , Espectrometria de Massas em Tandem , Animais , Crustáceos/química , Crustáceos/metabolismo , Peixes/metabolismo , Metanol , Nitrofuranos/química , Nitrofuranos/metabolismo , Reprodutibilidade dos Testes , Espectrometria de Massas em Tandem/métodosRESUMO
An accurate, reliable and fast multi-residue, multi-class method using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed and validated for simultaneous determination and quantification of 24 pharmacologically active substances of three different classes (Quinolones including fluoroquinolones, sulphonamides and tetracyclines) in aquaculture shrimps. Sample preparation involves extraction with acetonitrile containing 0.1% formic acid and followed by clean up with n-hexane and 0.1% methanol in water by UPLC-MS/MS within 8â¯min. The method was validated according to European Commission Decision 2002/657. Acceptable values were obtained for linearity (5-200⯵gâ¯kg-1), specificity, Limit of Quantification (5-10⯵gâ¯kg-1), recovery (between 83 and 100%), repeatability (RSDâ¯<â¯9%), within lab reproducibility (RSDâ¯<â¯15%), reproducibility (RSDâ¯≤â¯22%), decision limit (105-116⯵gâ¯kg-1) and detection capability (110-132⯵gâ¯kg-1). The validated method was applied to aquaculture shrimp samples from India.