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dc.contributor.authorDi Rocco, Melissa
dc.contributor.authorMoloney, Mary
dc.contributor.authorHaren, Deirdre
dc.contributor.authorGutierrez, Montserrat
dc.contributor.authorEarley, Seán
dc.contributor.authorBerendsen, Bjorn
dc.contributor.authorFurey, Ambrose
dc.contributor.authorDanaher, Martin
dc.date.accessioned2021-07-26T10:03:11Z
dc.date.available2021-07-26T10:03:11Z
dc.date.issued2020-05-23
dc.identifier.citationDi Rocco, M., Moloney, M., Haren, D. et al. Improving the chromatographic selectivity of β-lactam residue analysis in milk using phenyl-column chemistry prior to detection by tandem mass spectrometry. Anal Bioanal Chem 412, 4461–4475 (2020). https://doi.org/10.1007/s00216-020-02688-4en_US
dc.identifier.issn1618-2642
dc.identifier.urihttp://hdl.handle.net/11019/2501
dc.descriptionpeer-revieweden_US
dc.description.abstractAnalyte isobaric interferences can limit the development of a comprehensive analytical method for the quantitative liquid chromatography-tandem mass spectrometry profiling of an important cohort of veterinary drugs. In this work, a selective chromatographic separation was developed for the analysis of 32 β-lactam antibiotic residues (12 penicillins, 14 cephalosporins, five carbapenems and faropenem) in milk samples. A range of analytical columns with different stationary phases and mobile phases were evaluated for retention and separation of the β-lactam compounds. Results showed that, among the columns tested, only phenyl-hexyl could adequately separate ampicillin from cephalexin and amoxicillin from cefadroxil, which had shown isobaric interferences on a number of stationary phases. Chromatography was performed using a water/acetonitrile binary gradient with formic acid and ammonium acetate. The β-lactam residues were extracted from the milk samples using a water:acetonitrile solution and purified by C18 dispersive solid-phase extraction (d-SPE) clean-up, followed by concentration under nitrogen and ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) determination. Analytes were monitored in positive electrospray ionisation mode (ESI(+)). Possible interfering matrix effects were overcome by using 13 internal standards. The method was fully validated according to 2002/657/EC guidelines, showing satisfactory performance characteristics. Under within-laboratory reproducibility conditions, trueness and precision ranged from 91 to 130% and from 1.4 to 38.6%, respectively. Decision limits (CCα) were in the range 2.1–133 μg kg−1. Limits of detection (LODs) and quantitation (LOQs) ranged between 0.0090 and 1.5 μg kg−1 and from 0.030 to 5.0 μg kg−1, respectively.en_US
dc.description.sponsorshipThe FIRM programme administered by the Irish Department of Agriculture, Food and the Marine
dc.language.isoenen_US
dc.publisherSpringer Science and Business Media LLCen_US
dc.relation.ispartofseriesAnalytical and Bioanalytical Chemistry volume;vol 412
dc.rightsAttribution-NonCommercial-ShareAlike 4.0 International*
dc.rights.urihttps://www.springer.com/tdm
dc.rights.urihttp://creativecommons.org/licenses/by-nc-sa/4.0/*
dc.subjectBovine milken_US
dc.subjectChromatographic selectivityen_US
dc.subjectPhenyl-hexylen_US
dc.subjectUHPLC-MS/MSen_US
dc.subjectβ-Lactam antibioticsen_US
dc.titleImproving the chromatographic selectivity of β-lactam residue analysis in milk using phenyl-column chemistry prior to detection by tandem mass spectrometryen_US
dc.typeArticleen_US
dc.identifier.doihttps://doi.org/10.1007/s00216-020-02688-4
dc.identifier.pii2688
dc.contributor.sponsorDepartment of Agriculture, Food and the Marineen_US
dc.contributor.sponsorGrantNumber13/F484en_US
dc.source.volume412
dc.source.issue18
dc.source.beginpage4461
dc.source.endpage4475
refterms.dateFOA2021-07-26T10:03:12Z
dc.source.journaltitleAnalytical and Bioanalytical Chemistry
dc.identifier.eissn1618-2650


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