title: In-house validation of a liquid chromatography/electrospray tandem mass spectrometry method for confirmation of chloramphenicol residues in muscle according to Decision 2002/657/EC.
abstract: In this work we present an in-house validation study for the confirmatory analysis of chloramphenicol (CAP) in muscle according to the Commission Decision 2002/657/EC requirements. CAP is extracted in acetonitrile and after liquid-liquid partitioning with n-hexane is identified and quantitatively determined by ion trap liquid chromatography/electrospray ionisation tandem mass spectrometry (LC/ESI-MS/MS) analysis in the negative ion mode. CAP was identified using the precursor ion and at least two product ions, meeting the qualitative and quantitative criteria set by the European Commission in the Decision 2002/657/EC for confirmation of prohibited veterinary drug residues. We calculated mean drug recoveries, CCalpha and CCbeta of the method, and reported data on specificity, ruggedness and within-laboratory reproducibility. Finally, we point out and discuss some problems and questions arising from controversy about the application of Decision 2002/657/EC.
authors.affiliation: Istituto Zooprofilattico Sperimentale del Mezzogioro, via Salute 2, 80055 Portici (NA), Italy.
authors.forename: Floriana
authors.initials: F
authors.lastname: Vinci
authors.forename: Grazia
authors.initials: G
authors.lastname: Guadagnuolo
authors.forename: Vincenzo
authors.initials: V
authors.lastname: Danese
authors.forename: Marco
authors.initials: M
authors.lastname: Salini
authors.forename: Luigi
authors.initials: L
authors.lastname: Serpe
authors.forename: Pasquale
authors.initials: P
authors.lastname: Gallo
mesh_terms: D000818:Animals; D002701:Chloramphenicol / Q000032:analysis*; D002853:Chromatography, Liquid / Q000592:standards*; D007880:Legislation, Drug; D009132:Muscles / Q000737:chemistry*; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000592:standards*
chemical_list: D002701:Chloramphenicol