title: Determination of sulfonamide antibiotics and metabolites in liver, muscle and kidney samples by pressurized liquid extraction or ultrasound-assisted extraction followed by liquid chromatography-quadrupole linear ion trap-tandem mass spectrometry (HPLC-QqLIT-MS/MS).
abstract: Sulfonamides are widely used in human and veterinary medicine. The presence of sulfonamides residues in food is an issue of great concern. Throughout the present work, a method for the targeted analysis of 16 sulfonamides and metabolites residue in liver of several species has been developed and validated. Extraction and clean-up has been statistically optimized using central composite design experiments. Two extraction methods have been developed, validated and compared: i) pressurized liquid extraction, in which samples were defatted with hexane and subsequently extracted with acetonitrile and ii) ultrasound-assisted extraction with acetonitrile and further liquid-liquid extraction with hexane. Extracts have been analyzed by liquid chromatography-quadrupole linear ion trap-tandem mass spectrometry. Validation procedure has been based on the Commission Decision 2002/657/EC and included the assessment of parameters such as decision limit (CCα), detection capability (CCβ), sensitivity, selectivity, accuracy and precision. Method׳s performance has been satisfactory, with CCα values within the range of 111.2-161.4 µg kg(-1), limits of detection of 10 µg kg(-1) and accuracy values around 100% for all compounds.
authors.affiliation: Instituto de Química, Universidade Federal do Rio Grande do Sul - UFRGS, Avenida Bento Gonçalves, 6500 Porto Alegre, RS, Brazil; Laboratório Nacional Agropecuário - LANAGRO/RS, Estrada da Ponta Grossa, 3036 Porto Alegre, RS, Brazil. Electronic address: hoff@agricultura.gov.br.
authors.forename: Rodrigo Barcellos
authors.initials: RB
authors.lastname: Hoff
authors.affiliation: Instituto de Química, Universidade Federal do Rio Grande do Sul - UFRGS, Avenida Bento Gonçalves, 6500 Porto Alegre, RS, Brazil.
authors.forename: Tânia Mara
authors.initials: TM
authors.lastname: Pizzolato
authors.affiliation: Instituto de Química, Universidade Federal do Rio Grande do Sul - UFRGS, Avenida Bento Gonçalves, 6500 Porto Alegre, RS, Brazil.
authors.forename: Maria do Carmo Ruaro
authors.initials: MDCR
authors.lastname: Peralba
authors.affiliation: Department of Environmental Chemistry, IDAEA-CSIC, Jordi Girona 18-26, 08034 Barcelona, Spain.
authors.forename: M Silvia
authors.initials: MS
authors.lastname: Díaz-Cruz
authors.affiliation: Department of Environmental Chemistry, IDAEA-CSIC, Jordi Girona 18-26, 08034 Barcelona, Spain; Catalan Institute for Water Research (ICRA), Parc Científic i Tecnològic de la Universitat de Girona, C/Emili Grahit, 101 Edifici H2O, E-17003 Girona, Spain.
authors.forename: Damià
authors.initials: D
authors.lastname: Barceló
mesh_terms: D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D002645:Chickens; D002851:Chromatography, High Pressure Liquid; D005399:Fishes; D005506:Food Contamination / Q000032:analysis*; D059022:Food Safety; D006736:Horses; D007668:Kidney / Q000737:chemistry*; D059625:Liquid-Liquid Extraction; D008099:Liver / Q000737:chemistry*; D009132:Muscles / Q000737:chemistry*; D011312:Pressure; D015203:Reproducibility of Results; D012756:Sheep; D013449:Sulfonamides / Q000032:analysis*; D053719:Tandem Mass Spectrometry; D014465:Ultrasonics
chemical_list: D000900:Anti-Bacterial Agents; D013449:Sulfonamides
keywords: Central composite design; Food analysis; Metabolites; Pressurized liquid extraction; Sulfonamides; Ultrasound-assisted extraction; Veterinary drugs