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.
Assuntos
Antibacterianos/análise , Cromatografia Líquida de Alta Pressão/métodos , Contaminação de Alimentos/análise , Frutos do Mar/análise , Espectrometria de Massas em Tandem/métodos , Acetonitrilas/química , Animais , Aquicultura , Decápodes/química , Fluoroquinolonas/análise , Índia , Limite de Detecção , Quinolonas/análise , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Sulfonamidas/análise , Tetraciclinas/análiseRESUMO
This study enables the selective determination of inorganic arsenic (iAs) with a low detection limit using an economical instrument [atomic absorption spectrometer with hydride generation (HG)] to meet the regulatory requirements as per European Commission (EC) and Codex guidelines. Dry rice samples (0.5 g) were diluted using 0.1 M HNO3-3% H2O2 and heated in a water bath (90 ± 2°C) for 60 min. Through this process, all the iAs is solubilized and oxidized to arsenate [As(V)]. The centrifuged extract was loaded onto a preconditioned and equilibrated strong anion-exchange SPE column (silica-based Strata SAX 500 mg/6 mL), followed by selective and sequential elution of As(V), enabling the selective quantification of iAs using atomic absorption spectrometry with HG. In-house validation showed a mean recovery of 94% and an LOQ of 0.025 mg/kg. The repeatability (HorRatr) and reproducibility (HorRatR) values were <2, meeting the performance criteria mandated by the EC. The combined standard measurement uncertainty by this method was less than the maximum standard measurement uncertainty; thus, the method can be considered for official control purposes. The method was applied for the determination of iAs in husked rice samples and has potential applications in other food commodities.