title: Screening and confirmatory method for multiclass determination of 62 antibiotics in meat.
abstract: A multiclass method for screening and confirmatory analysis of antimicrobial residues in muscle has been developed and validated, according to Commission Decision 2002/657/EC. Sixty-two antibiotics belonging to ten different drug families (amphenicols, beta-lactams, diamino-pyrimidine, lincosamides, macrolides, pleuromutilins, quinolones, rifamycins, sulfonamides and tetracyclines) have been included in the method. After the addition of an aqueous solution of EDTA, the minced muscle was extracted with acetonitrile/water mixture and, later, with pure acetonitrile. The extract was evaporated and redissolved in ammonium acetate buffer prior to LC injection. Instrumental determination was performed by liquid chromatography coupled to hybrid high resolution mass analyser (LC-HRMS/MS) operating in positive electrospray ionization mode. Chromatographic separation was optimized on a Poroshell 120 EC-C18 column (100 × 3.0 mm, 2.7 μm) with gradient using methanol and water containing 0.1% of formic acid as mobile phases. The method was validated in bovine muscle in the range 3.3-150 μg kg(-1) for all antibiotics; for some compounds with MRL higher than 100 μg kg(-1), the validation interval has been extended until 1500 μg kg(-1). The studied performance characteristics were selectivity, linearity, precision, trueness (recovery), decision limits, detection capabilities, detection and quantification limits. Satisfactory quantitative performances were obtained for all the analytes. Ruggedness tests demonstrated the applicability to swine and poultry muscle, too. Finally the wide participation in proficiency tests allowed to investigate in deep the method performances.
authors.affiliation: Istituto Zooprofilattico Sperimentale dell'Umbria e delle Marche, Via G. Salvemini, 1, 06126 Perugia, Italy.
authors.forename: Simone
authors.initials: S
authors.lastname: Moretti
authors.affiliation: Istituto Zooprofilattico Sperimentale della Lombardia e dell'Emilia Romagna "B. Ubertini", Via A. Bianchi, 7/9, 25124 Brescia, Italy.
authors.forename: Guglielmo
authors.initials: G
authors.lastname: Dusi
authors.affiliation: Istituto Zooprofilattico Sperimentale dell'Umbria e delle Marche, Via G. Salvemini, 1, 06126 Perugia, Italy.
authors.forename: Danilo
authors.initials: D
authors.lastname: Giusepponi
authors.affiliation: Istituto Zooprofilattico Sperimentale della Lombardia e dell'Emilia Romagna "B. Ubertini", Via A. Bianchi, 7/9, 25124 Brescia, Italy.
authors.forename: Simona
authors.initials: S
authors.lastname: Pellicciotti
authors.affiliation: Istituto Zooprofilattico Sperimentale dell'Umbria e delle Marche, Via G. Salvemini, 1, 06126 Perugia, Italy.
authors.forename: Rosanna
authors.initials: R
authors.lastname: Rossi
authors.affiliation: Istituto Zooprofilattico Sperimentale dell'Umbria e delle Marche, Via G. Salvemini, 1, 06126 Perugia, Italy.
authors.forename: Giorgio
authors.initials: G
authors.lastname: Saluti
authors.affiliation: Department of Chemistry, Biology and Biotechnology, University of Perugia, Via Elce di Sotto 10, 06123 Perugia, Italy.
authors.forename: Gabriele
authors.initials: G
authors.lastname: Cruciani
authors.affiliation: Istituto Zooprofilattico Sperimentale dell'Umbria e delle Marche, Via G. Salvemini, 1, 06126 Perugia, Italy. Electronic address: r.galarini@izsum.it.
authors.forename: Roberta
authors.initials: R
authors.lastname: Galarini
mesh_terms: D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D002417:Cattle; D002853:Chromatography, Liquid; D004350:Drug Residues / Q000032:analysis; D005504:Food Analysis / Q000379:methods*; D018942:Macrolides / Q000032:analysis; D008460:Meat / Q000032:analysis*; D009132:Muscles / Q000737:chemistry; D015363:Quinolones / Q000032:analysis; D013449:Sulfonamides / Q000032:analysis; D013552:Swine; D013754:Tetracyclines / Q000032:analysis; D047090:beta-Lactams / Q000032:analysis
chemical_list: D000900:Anti-Bacterial Agents; D018942:Macrolides; D015363:Quinolones; D013449:Sulfonamides; D013754:Tetracyclines; D047090:beta-Lactams
keywords: Antibiotics; Liquid chromatography high resolution mass spectrometry; Method validation; Muscle