title: LC-MS/MS methods for sulfadimethoxine and ormetoprim analysis in feed and fish fillet and a leaching study for feed after alternative procedures for the incorporation of drugs.
abstract: This paper describes the method development for sulfadimethoxine (SDM) and ormetoprim (OMP) quantitation in fish feed and fish fillet employing LC-MS/MS. In order to assess the reliability of the analytical method, valuation was undertaken as recommended by guidelines proposed by the Brazilian Ministry of Agriculture. The calibration curve for the quantification of both drugs in feed showed adequate linearity (r > 0.99), precision (CV < 12%) and trueness ranging from 97% to 100%. The method for the determination of SDM and OMP residues in fish fillet involved a simple sample preparation procedure that had adequate linearity (r > 0.99), precision (CV < 16%) and trueness around 100%, with CCα < 100.2 ng g-1and CCβ < 100.4 ng g-1. With a goal of avoiding the risk of drug leaching from feed into the aquatic environment during fish medication via the oral route, different procedures for drug incorporation into feed were evaluated. Coating feed pellets with ethyl cellulose polymer containing the drug showed promising results. In this case, medicated feed released drugs to water at a level below 6% when the medicated feed stayed in the water for up to 15 min.
authors.affiliation: a School of Pharmaceutical Sciences of Ribeirão Preto, Department of Physics and Chemistry , University of São Paulo , Ribeirão Preto/SP , Brazil.
authors.forename: Ana Paula
authors.initials: AP
authors.lastname: Fais
authors.affiliation: a School of Pharmaceutical Sciences of Ribeirão Preto, Department of Physics and Chemistry , University of São Paulo , Ribeirão Preto/SP , Brazil.
authors.forename: Rodolfo Scarpino Barboza
authors.initials: RS
authors.lastname: Franco
authors.affiliation: a School of Pharmaceutical Sciences of Ribeirão Preto, Department of Physics and Chemistry , University of São Paulo , Ribeirão Preto/SP , Brazil.
authors.forename: Agnaldo Fernando Baldo
authors.initials: AF
authors.lastname: da Silva
authors.affiliation: b School of Pharmaceutical Sciences of Ribeirão Preto, Department of Pharmaceutical Sciences , University of São Paulo , Ribeirão Preto/SP , Brazil.
authors.forename: Osvaldo
authors.initials: O
authors.lastname: de Freitas
authors.affiliation: a School of Pharmaceutical Sciences of Ribeirão Preto, Department of Physics and Chemistry , University of São Paulo , Ribeirão Preto/SP , Brazil.
authors.forename: Jonas Augusto Rizzato
authors.initials: JA
authors.lastname: Paschoal
mesh_terms: D000821:Animal Feed / Q000032:analysis*; D000818:Animals; D000890:Anti-Infective Agents / Q000008:administration & dosage / Q000032:analysis* / Q000378:metabolism; D001711:Biotransformation; D001938:Brazil; D002482:Cellulose / Q000031:analogs & derivatives / Q000737:chemistry; D060125:Characiformes; D002853:Chromatography, Liquid; D020099:Coated Materials, Biocompatible / Q000737:chemistry; D065546:Drug Liberation; D004350:Drug Residues / Q000032:analysis* / Q000378:metabolism; D017408:Guidelines as Topic; D006801:Humans; D007700:Kinetics; D057230:Limit of Detection; D059625:Liquid-Liquid Extraction / Q000379:methods; D008460:Meat / Q000032:analysis*; D011743:Pyrimidines / Q000008:administration & dosage / Q000032:analysis* / Q000378:metabolism; D013412:Sulfadimethoxine / Q000008:administration & dosage / Q000032:analysis* / Q000378:metabolism; D053719:Tandem Mass Spectrometry
chemical_list: D000890:Anti-Infective Agents; D020099:Coated Materials, Biocompatible; D011743:Pyrimidines; D013412:Sulfadimethoxine; C013517:ethyl cellulose; D002482:Cellulose; C100125:ormetoprim
keywords: Food contaminants; LC-MS/MS; antimicrobial drugs; aquaculture; ormetoprim; sulfadimethoxine; veterinary drug residues