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

• Published in: Rapid communications in mass spectrometry 2005-01, Vol.19 (22), p.3349-3355
• Main Authors: Vinci, Floriana, Guadagnuolo, Grazia, Danese, Vincenzo, Salini, Marco, Serpe, Luigi, Gallo, Pasquale
• Format: Article
• Language: English
• Subjects: Animals; Chloramphenicol - analysis; Chromatography, Liquid - standards; Legislation, Drug; Muscles - chemistry; Reproducibility of Results; Spectrometry, Mass, Electrospray Ionization - standards
• ISSN: 0951-4198; 1097-0231
• DOI: 10.1002/rcm.2200

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, CCα and CCβ 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. Copyright © 2005 John Wiley & Sons, Ltd.