Validation of a liquid chromatography–electrospray ionization tandem mass spectrometric method to determine six polyether ionophores in raw, UHT, pasteurized and powdered milk

•Use of different kinds of processed milk, besides raw milk, during validation.•Sample variability considered in validation raises odds of routine reliable results.•The validated method does not include a SPE clean-up step.•A QuEChERS extraction is used in the proposed method.•Six polyether ionophor...

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Veröffentlicht in:Food chemistry 2016-04, Vol.196, p.130-137
Hauptverfasser: Pereira, Mararlene Ulberg, Spisso, Bernardete Ferraz, Jacob, Silvana do Couto, Monteiro, Mychelle Alves, Ferreira, Rosana Gomes, Carlos, Betânia de Souza, da Nóbrega, Armi Wanderley
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Sprache:eng
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Zusammenfassung:•Use of different kinds of processed milk, besides raw milk, during validation.•Sample variability considered in validation raises odds of routine reliable results.•The validated method does not include a SPE clean-up step.•A QuEChERS extraction is used in the proposed method.•Six polyether ionophores can be simultaneously determined in milk. This study aimed to validate a method developed for the determination of six antibiotics from the polyether ionophore class (lasalocid, maduramicin, monensin, narasin, salinomycin and semduramicin) at residue levels in raw, UHT, pasteurized and powdered milk using QuEChERS extraction and high performance liquid chromatography coupled to tandem mass spectrometry (HPLC–MS/MS). The validation was conducted under an in-house laboratory protocol that is primarily based on 2002/657/EC Decision, but takes in account the variability of matrix sources. Overall recoveries between 93% and 113% with relative standard deviations up to 16% were obtained under intermediate precision conditions. CCα calculated values did not exceed 20% the Maximum Residue Limit for monensin and 25% the Maximum Levels for all other substances. The method showed to be simple, fast and suitable for verifying the compliance of raw and processed milk samples regarding the limits recommended by Codex Alimentarius and those adopted in European Community for polyether ionophores.
ISSN:0308-8146
1873-7072
DOI:10.1016/j.foodchem.2015.09.011