title: Simple confirmatory assay for analyzing residues of aminoglycoside antibiotics in bovine milk: hot water extraction followed by liquid chromatography-tandem mass spectrometry.
abstract: A simple, selective and sensitive procedure for determining nine widely used aminoglycoside antibiotics (AGs) in bovine whole milk is presented. It is based on matrix solid-phase dispersion with heated water, at 70 degrees C, as extractant followed by liquid chromatography (LC)-tandem mass spectrometry (MS) using an electrospray ion source. After acidification and filtration, 0.2 ml of the aqueous extract was injected into the LC column. MS data acquisition was performed in the multi reaction monitoring mode, selecting two (three, when possible) precursor ion > product ion transitions for each target compound. Analyte recoveries ranged between 70 and 92%. Using aminosidine (an AG not used in veterinary medicine) as surrogate internal standard, the accuracy of the method at three spike levels varied between 80 and 107% with R.S.D. not larger than 11%. The limits of quantification were between 2 ng/ml (apramycin) and 13 ng/ml (streptomycin). They are well below the tolerance levels set by both the European Union and the U.S. Food and Drug Administration.
authors.affiliation: Dipartimento di Chimica, Università "La Sapienza", Piazza Aldo Moro 5, 00185 Roma, Italy.
authors.forename: Sara
authors.initials: S
authors.lastname: Bogialli
authors.forename: Roberta
authors.initials: R
authors.lastname: Curini
authors.forename: Antonio
authors.initials: A
authors.lastname: Di Corcia
authors.forename: Aldo
authors.initials: A
authors.lastname: Laganà
authors.forename: Monica
authors.initials: M
authors.lastname: Mele
authors.forename: Manuela
authors.initials: M
authors.lastname: Nazzari
mesh_terms: D000617:Aminoglycosides / Q000032:analysis*; D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D002417:Cattle; D002853:Chromatography, Liquid / Q000379:methods*; D008892:Milk / Q000737:chemistry*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
chemical_list: D000617:Aminoglycosides; D000900:Anti-Bacterial Agents