title: Determination and confirmation of chloramphenicol in honey, fish and prawns by liquid chromatography-tandem mass spectrometry with minimum sample preparation: validation according to 2002/657/EC Directive.
abstract: A reliable, simple and sensitive liquid chromatography-electrospray ionisation-tandem mass spectrometry (LC-ESI-MS/MS) confirmation method has been developed for chloramphenicol (CAP) determination in honey, fish and prawns. For honey, samples were extracted with ethyl acetate, an aliquot was evaporated to dryness and re-dissolved in mobile phase. For fish and prawns, tissues were extracted with acetonitrile and chloroform. The organic layer was evaporated to dryness and the residue was re-constituted with water: acetonitrile (90:10). LC separation was achieved on a C18 column with gradient elution using a mobile phase of acetonitrile and water. Analysis was carried out on a triple-quadrupole tandem mass spectrometer in multiple reaction monitoring (MRM) mode via electrospray interface operated in negative ionisation mode, with deuterated chloramphenicol-d(5) (d(5)-CAP) as internal standard. Method validation was performed according to the criteria of Commission Decision 2002/657/EC. Four identification points were obtained for CAP with one precursor ion and two product ions. The limit of detection (LOD) was 0.02 µg kg(-1). Linear calibration curves were obtained over concentration ranges of 0.1-1.0 µg kg(-1) in tissues. Mean recoveries ranged from 85.5% to 115.6%, with the corresponding intra- and inter-day variation ranging from 1.0% to 22.5%, depending on matrix type and level of concentration. The decision limit (CCα) and detection capability (CCβ) of the method were obtained for all matrices: 0.04 and 0.06 µg kg(-1), respectively, for prawns and fish and 0.05 and 0.09 µg kg(-1) for honey.
authors.affiliation: Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Nacional Agropecuário - LANAGRO/RS, Porto Alegre, RS, Brazil. fabiano.barreto@agricultura.gov.br
authors.forename: Fabiano
authors.initials: F
authors.lastname: Barreto
authors.forename: Cristina
authors.initials: C
authors.lastname: Ribeiro
authors.forename: Rodrigo Barcellos
authors.initials: RB
authors.lastname: Hoff
authors.forename: Teresa Dalla
authors.initials: TD
authors.lastname: Costa
mesh_terms: D000818:Animals; D002701:Chloramphenicol / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis*; D005062:European Union; D005399:Fishes; D005506:Food Contamination / Q000032:analysis* / Q000331:legislation & jurisprudence / Q000706:statistics & numerical data; D006722:Honey / Q000032:analysis; D057230:Limit of Detection; D017747:Seafood / Q000032:analysis; D012758:Shellfish / Q000032:analysis; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods*; D019155:Veterinary Drugs / Q000032:analysis
chemical_list: D019155:Veterinary Drugs; D002701:Chloramphenicol