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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

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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-d5 (d5-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.
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Keywords: LC/MS; chloramphenicol; chromatographic analysis; clean-up; fish and fish products; honey; meat

Document Type: Research Article

Affiliations: 1: Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Nacional Agropecuário – LANAGRO/RS, Porto Alegre,RS, Brazil 2: Programa de Pós-Graduação em Ciências Farmacêuticas, Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul, Porto Alegre,RS, Brazil

Publication date: April 1, 2012

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