title: Validation of a liquid chromatography-electrospray ionization tandem mass spectrometric method to determine six polyether ionophores in raw, UHT, pasteurized and powdered milk.
abstract: 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.
authors.affiliation: National Institute for Quality Control in Health/Oswaldo Cruz Foundation (INCQS/FIOCRUZ), Av. Brasil 4365, Rio de Janeiro, RJ, Brazil. Electronic address: mararlene.pereira@incqs.fiocruz.br.
authors.forename: Mararlene Ulberg
authors.initials: MU
authors.lastname: Pereira
authors.affiliation: National Institute for Quality Control in Health/Oswaldo Cruz Foundation (INCQS/FIOCRUZ), Av. Brasil 4365, Rio de Janeiro, RJ, Brazil.
authors.forename: Bernardete Ferraz
authors.initials: BF
authors.lastname: Spisso
authors.affiliation: National Institute for Quality Control in Health/Oswaldo Cruz Foundation (INCQS/FIOCRUZ), Av. Brasil 4365, Rio de Janeiro, RJ, Brazil.
authors.forename: Silvana do Couto
authors.initials: Sdo C
authors.lastname: Jacob
authors.affiliation: National Institute for Quality Control in Health/Oswaldo Cruz Foundation (INCQS/FIOCRUZ), Av. Brasil 4365, Rio de Janeiro, RJ, Brazil.
authors.forename: Mychelle Alves
authors.initials: MA
authors.lastname: Monteiro
authors.affiliation: National Institute for Quality Control in Health/Oswaldo Cruz Foundation (INCQS/FIOCRUZ), Av. Brasil 4365, Rio de Janeiro, RJ, Brazil.
authors.forename: Rosana Gomes
authors.initials: RG
authors.lastname: Ferreira
authors.affiliation: National Institute for Quality Control in Health/Oswaldo Cruz Foundation (INCQS/FIOCRUZ), Av. Brasil 4365, Rio de Janeiro, RJ, Brazil.
authors.forename: Betânia de Souza
authors.initials: Bde S
authors.lastname: Carlos
authors.affiliation: National Institute for Quality Control in Health/Oswaldo Cruz Foundation (INCQS/FIOCRUZ), Av. Brasil 4365, Rio de Janeiro, RJ, Brazil.
authors.forename: Armi Wanderley
authors.initials: AW
authors.lastname: da Nóbrega
mesh_terms: D000818:Animals; D002853:Chromatography, Liquid / Q000379:methods*; D007476:Ionophores / Q000737:chemistry*; D008892:Milk / Q000737:chemistry*; D061352:Pasteurization; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D007476:Ionophores
keywords: Anticoccidials; Coccidiostats; Ionophores; LC–MS/MS; Lasalocid A sodium salt (PubChem CID: 2724110); Maduramicin alpha ammonium salt (PubChem CID: 68595); Milk; Monensin A sodium salt hydrate (PubChem CID: 71312633); Narasin A (PubChem CID: 65452); Nigericin sodium salt (PubChem CID: 23681158); QuEChERS; Salinomycin A (PubChem CID: 3085092); Semduramicin sodium (PubChem CID: 23678834); Veterinary drug residues