title: Development of a liquid chromatography/electrospray tandem mass spectrometry method for confirmation of chloramphenicol residues in milk after alfa-1-acid glycoprotein affinity chromatography.
abstract: In this work we present a method for confirmatory analysis of chloramphenicol (CAP) in bovine and buffalo raw milk. CAP is extracted in acetonitrile and purified by affinity chromatography on an alpha-1-acid glycoprotein (AAG) column, then is identified and determined by ion-trap liquid chromatography/electrospray ionisation tandem mass spectrometry (LC/ESI-MS/MS) analysis in the negative ion mode. CAP was identified at the minimum required performance limit (MRPL) of 0.30 ppb, by monitoring the [M-H]- ion and at least two product ions, meeting the qualitative and quantitative criteria set by the European Commission in Decision 2002/657/EC for confirmation of prohibited veterinary drugs. The trueness and within-day and between-day repeatability data are also reported. Moreover, the loading capacity of affinity columns towards CAP was tested. This method, based on the molecular recognition between drug and AAG during the purification step to improve sample cleanup, represents a quantitative and repeatable procedure for confirmatory analysis, and fits the requirements for the routine official control of CAP residues in raw milk.
authors.affiliation: Istituto Zooprofilattico Sperimentale del Mezzogiorno, via Salute 2, 80055 Portici (NA), Italy. p.gallo@izsmportici.it
authors.forename: Pasquale
authors.initials: P
authors.lastname: Gallo
authors.forename: Antonella
authors.initials: A
authors.lastname: Nasi
authors.forename: Floriana
authors.initials: F
authors.lastname: Vinci
authors.forename: Grazia
authors.initials: G
authors.lastname: Guadagnuolo
authors.forename: Gianfranco
authors.initials: G
authors.lastname: Brambilla
authors.forename: Maurizio
authors.initials: M
authors.lastname: Fiori
authors.forename: Luigi
authors.initials: L
authors.lastname: Serpe
mesh_terms: D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D002417:Cattle; D002701:Chloramphenicol / Q000032:analysis*; D002846:Chromatography, Affinity / Q000379:methods*; D004350:Drug Residues / Q000032:analysis; D005062:European Union; D005260:Female; D005506:Food Contamination / Q000032:analysis / Q000331:legislation & jurisprudence / Q000517:prevention & control; D008892:Milk / Q000737:chemistry*; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D019155:Veterinary Drugs / Q000032:analysis
chemical_list: D000900:Anti-Bacterial Agents; D019155:Veterinary Drugs; D002701:Chloramphenicol