title: A simple, fast and cheap non-SPE screening method for antibacterial residue analysis in milk and liver using liquid chromatography-tandem mass spectrometry.
abstract: In routine laboratory work, screening methods for multiclass analysis can process a large number of samples in a short time. The main challenge is to develop a methodology to detect as many different classes of residues as possible, combined with speed and low cost. An efficient technique for the analysis of multiclass antibacterial residues (fluoroquinolones, tetracyclines, sulfonamides and trimethoprim) was developed based on simple, environment-friendly extraction for bovine milk, cattle and poultry liver. Acidified ethanol was used as an extracting solvent for milk samples. Liver samples were treated using EDTA-washed sand for cell disruption, methanol:water and acidified acetonitrile as extracting solvent. A total of 24 antibacterial residues were detected and confirmed using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS), at levels between 10, 25 and 50% of the maximum residue limit (MRL). For liver samples a metabolite (sulfaquinoxaline-OH) was also monitored. A validation procedure was conducted for screening purposes in accordance with European Union requirements (2002/657/EC). The detection capability (CCβ) false compliant rate was less than 5% at the lowest level for each residue. Specificity and ruggedness were also discussed. Incurred and routine samples were analyzed and the method was successfully applied. The results proved that this method can be an important tool in routine analysis, since it is very fast and reliable.
authors.affiliation: Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Nacional Agropecuário-LANAGRO/RS, Porto Alegre, RS, Brazil; Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul, Porto Alegre, RS, Brazil. Electronic address: magdatm@terra.com.br.
authors.forename: Magda Targa
authors.initials: MT
authors.lastname: Martins
authors.affiliation: Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Nacional Agropecuário-LANAGRO/RS, Porto Alegre, RS, Brazil.
authors.forename: Jéssica
authors.initials: J
authors.lastname: Melo
authors.affiliation: Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Nacional Agropecuário-LANAGRO/RS, Porto Alegre, RS, Brazil; Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul, Porto Alegre, RS, Brazil.
authors.forename: Fabiano
authors.initials: F
authors.lastname: Barreto
authors.affiliation: Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Nacional Agropecuário-LANAGRO/RS, Porto Alegre, RS, Brazil; Instituto de Química, Universidade Federal do Rio Grande do Sul, Porto Alegre, RS, Brazil.
authors.forename: Rodrigo Barcellos
authors.initials: RB
authors.lastname: Hoff
authors.affiliation: Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Nacional Agropecuário-LANAGRO/RS, Porto Alegre, RS, Brazil; Instituto de Química, Universidade Federal do Rio Grande do Sul, Porto Alegre, RS, Brazil.
authors.forename: Louise
authors.initials: L
authors.lastname: Jank
authors.affiliation: Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Nacional Agropecuário-LANAGRO/RS, Porto Alegre, RS, Brazil.
authors.forename: Michele Soares
authors.initials: MS
authors.lastname: Bittencourt
authors.affiliation: Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Nacional Agropecuário-LANAGRO/RS, Porto Alegre, RS, Brazil; Instituto de Química, Universidade Federal do Rio Grande do Sul, Porto Alegre, RS, Brazil.
authors.forename: Juliana Bazzan
authors.initials: JB
authors.lastname: Arsand
authors.affiliation: Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul, Porto Alegre, RS, Brazil.
authors.forename: Elfrides Eva Scherman
authors.initials: EE
authors.lastname: Schapoval
mesh_terms: D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D002417:Cattle; D002853:Chromatography, Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis*; D000431:Ethanol / Q000737:chemistry; D024841:Fluoroquinolones / Q000032:analysis; D005504:Food Analysis / Q000379:methods*; D057230:Limit of Detection; D008099:Liver / Q000737:chemistry*; D000432:Methanol / Q000737:chemistry; D008892:Milk / Q000737:chemistry*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000379:methods; D012997:Solvents / Q000737:chemistry; D021241:Spectrometry, Mass, Electrospray Ionization; D013449:Sulfonamides / Q000032:analysis; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013754:Tetracyclines / Q000032:analysis; D014295:Trimethoprim / Q000032:analysis; D014867:Water / Q000737:chemistry
chemical_list: D000900:Anti-Bacterial Agents; D024841:Fluoroquinolones; D012997:Solvents; D013449:Sulfonamides; D013754:Tetracyclines; D014867:Water; D000431:Ethanol; D014295:Trimethoprim; D000432:Methanol
keywords: Antibacterials; LC–MS/MS; Liver; Milk; Residues