title: Determination of nitroimidazole residues in aquaculture tissue using ultra high performance liquid chromatography coupled to tandem mass spectrometry.
abstract: An UHPLC-MS/MS method was developed for the quantitative confirmatory analysis of residues of nitroimidazole drugs (dimetridazole, ipronidazole, metronidazole, ornidazole and ronidazole) and their corresponding hydroxy metabolites (HMMNI, ipronidazile-OH and metronidazole-OH) in aquaculture tissue. Samples were extracted by shaking in acetonitrile, water, MgSO4 and NaCl before being defatted with n-hexane pre-saturated with acetonitrile and concentrated under nitrogen. Nitroimidazole residues were determined by UHPLC-MS/MS operating in positive electrospray ionisation mode using a reversed phase BEH C18 column. The method was validated according to the EU Commission Decision 2002/657/EC guidelines. The following performance studies were carried out: specificity, selectivity, linearity, within laboratory repeatability (WLr)/reproducibility (WLR), accuracy, precision, decision limit (CCα), detection capability (CCβ), absolute recovery and stability. The analytical range of the method is 0.1-20 μg kg(-1). Accuracy and precision of the method, under within-laboratory reproducibility conditions, ranged from 83 to 105% and 2.3 to 14.0%, respectively. CCα were 0.07-1.0 μg kg(-1) depending on analyte and matrix. A total of 50 samples can be analysed in a single day using the assay. The method has been extensively evaluated through application to real test samples.
authors.affiliation: Food Safety Department, Teagasc Food Research Centre, Ashtown, Dublin 15, Ireland; Team Elucidate, Department of Chemistry, Cork Institute of Technology, Bishopstown, Cork, Ireland.
authors.forename: Anna
authors.initials: A
authors.lastname: Gadaj
authors.affiliation: Department of Life, Health and Environmental Sciences, University of L'Aquila, L'Aquila, Italy.
authors.forename: Valentina
authors.initials: V
authors.lastname: di Lullo
authors.affiliation: Food Safety Department, Teagasc Food Research Centre, Ashtown, Dublin 15, Ireland.
authors.forename: Helen
authors.initials: H
authors.lastname: Cantwell
authors.affiliation: Food Safety Department, Teagasc Food Research Centre, Ashtown, Dublin 15, Ireland.
authors.forename: Martin
authors.initials: M
authors.lastname: McCormack
authors.affiliation: Team Elucidate, Department of Chemistry, Cork Institute of Technology, Bishopstown, Cork, Ireland.
authors.forename: Ambrose
authors.initials: A
authors.lastname: Furey
authors.affiliation: Food Safety Department, Teagasc Food Research Centre, Ashtown, Dublin 15, Ireland. Electronic address: martin.danaher@teagasc.ie.
authors.forename: Martin
authors.initials: M
authors.lastname: Danaher
mesh_terms: D000818:Animals; D017756:Aquaculture; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis*; D005399:Fishes; D057230:Limit of Detection; D016014:Linear Models; D009593:Nitroimidazoles / Q000032:analysis*; D033561:Penaeidae; D015203:Reproducibility of Results; D017747:Seafood / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D009593:Nitroimidazoles
keywords: Aquaculture; Nitroimidazole residues; Prawn; Salmon; Sea bass; Shrimp; Tilapia; Trout; UHPLC-MS/MS