Evidence of non-extractable florfenicol residues: The development and validation of a confirmatory method for total florfenicol content in kidney by UPLC-MS/MS

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dc.contributor.authorFaulkner, Dermot V.
dc.contributor.authorCantley, Lynne M.
dc.contributor.authorWalker, Matthew
dc.contributor.authorCrooks, Steven
dc.date.accessioned2021-10-05T14:05:54Z
dc.date.available2021-10-05T14:05:54Z
dc.date.issued2016-05-20
dc.descriptionPublication history: Accepted - 27 March 2016; Published online - 20 May 2016.en_US
dc.description.abstractThe parent compound florfenicol (FF) is a broad-spectrum antibacterial compound licensed in the UK for use in cattle, pigs and the aquaculture industry. The analysis of porcine tissues in this study demonstrates that significant amounts of solvent non-extractable FF-related residues are present in incurred tissues (kidney and muscle) from treated animals. The results indicate that methods based on solvent extraction alone may carry a significant risk of reporting false-negative results. The use of a strong acid hydrolysis step prior to solvent extraction of tissue samples is necessary for an accurate estimate of the total tissue FF content. A robust and sensitive method for the determination of total FF residue content in kidney samples by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been developed and validated. This method covers the synthetic amphenicol drug FF and its metabolites, measured as the marker residue florfenicol amine (FFA) as per Commission Regulation (EU) No. 37/2010. Non-extractable and intermediate metabolites are converted to the hydrolysis product FFA, and then partitioned into ethyl acetate. Extracts are solvent exchanged prior to a dispersive solid-phase extraction step, then analysed using an alkaline reverse-phase gradient separation by UPLC-MS/MS. The method was validated around the maximum residue levels (MRLs) set out in Regulation (EU) No. 37/2010 for bovine kidney in accordance with Commission Decision No. 2002/657/EC. The following method performance characteristics were assessed during a single laboratory validation study: selectivity, specificity, sensitivity, linearity, matrix effects, accuracy and precision (decision limit (CCα) and detection capability (CCβ) were determined).en_US
dc.identifierhttp://hdl.handle.net/20.500.12518/356
dc.identifier.citationFaulkner, D., Cantley, M., Walker, M., Crooks, S., Kennedy, D. and Elliott, C. (2016) ‘Evidence of non-extractable florfenicol residues: development and validation of a confirmatory method for total florfenicol content in kidney by UPLC-MS/MS’, Food Additives & Contaminants: Part A. Informa UK Limited. doi:10.1080/19440049.2016.1175187en_US
dc.identifier.issn1944-0049
dc.identifier.issn1944-0057
dc.identifier.urihttps://doi.org/10.1080/19440049.2016.1175187
dc.language.isoenen_US
dc.publisherTaylor & Francisen_US
dc.rightsCopyright 2016, Informa UK Ltd, trading as Taylor & Francis Group. This work is made available online in accordance with the publisher's policies. Please refer to any applicable terms of use of the publisheren_US
dc.subjectFlorfenicol amineen_US
dc.subjectincurred tissueen_US
dc.subjectnon-extractableen_US
dc.subjectkidneyen_US
dc.subjectmuscleen_US
dc.subjecthydrolysisen_US
dc.subjectliquid chromatographyen_US
dc.subjectmass spectrometryen_US
dc.subjectUPLC-MS/MSen_US
dc.titleEvidence of non-extractable florfenicol residues: The development and validation of a confirmatory method for total florfenicol content in kidney by UPLC-MS/MSen_US
dc.typeArticleen_US
dcterms.dateAccepted2016-03-27
dcterms.dateSubmitted2016-01-21

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