title: A simple and high-throughput method for determination and confirmation of 14 coccidiostats in poultry muscle and eggs using liquid chromatography - quadrupole linear ion trap - tandem mass spectrometry (HPLC-QqLIT-MS/MS): Validation according to European Union 2002/657/EC.
abstract: A simple and fast quantitative and confirmatory multi-residue method was developed and validated for the determination of 14 coccidiostats residues in poultry muscle and eggs using liquid chromatography-tandem mass spectrometry (LC/MS-MS). The compounds were analyzed in a single run including lasalocid A, maduramicin, monensin, narasin, salinomycin, semduramicin, robenidine, diclazuril, toltrazuril, trimethoprim, clopidol, amprolium, diaveridine and nicarbazin (as the marker residue dinitrocarbanilide). A low-cost extraction and clean up procedure was optimized without the need of solid-phase extraction. Samples were extracted with acetonitrile followed by low-temperature clean up. Chromatographic separation was achieved using a C18 column, using water and acetonitrile, both containing 5mmolL-1of formic acid and 1mmolL-1ammonium acetate, as mobile phase. Coccidiostats were ionized in negative and positive mode and monitored simultaneously. The method was fully validated according with Commission Decision 2002/657/EC and was applied for >100 samples from the Brazilian National Residue Control Plan (NRCP). Parameters as precision, reproducibility, trueness, CCα and CCβ were determined. Trueness values were within the range 73-115%. Precision (repeatability and intermediate precision) ranged from 0.4% to 21% and intralaboratory reproducibility ranged from 6.3% to 27%, depending on matrix.
authors.affiliation: Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Nacional Agropecuário - MAPA/LANAGRO/RS, Porto Alegre, RS, Brazil; Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul, Porto Alegre, RS, Brazil. Electronic address: fabiano.barreto@agricultura.gov.br.
authors.forename: Fabiano
authors.initials: F
authors.lastname: Barreto
authors.affiliation: Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Nacional Agropecuário - MAPA/LANAGRO/RS, Porto Alegre, RS, Brazil.
authors.forename: Cristina
authors.initials: C
authors.lastname: Ribeiro
authors.affiliation: Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Nacional Agropecuário - MAPA/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: Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul, Porto Alegre, RS, Brazil.
authors.forename: Teresa Dalla
authors.initials: TD
authors.lastname: Costa
mesh_terms: D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003049:Coccidiostats / Q000032:analysis*; D004350:Drug Residues / Q000032:analysis*; D004531:Eggs / Q000032:analysis*; D005062:European Union; D057166:High-Throughput Screening Assays / Q000379:methods*; D009132:Muscles / Q000737:chemistry*; D011200:Poultry; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D003049:Coccidiostats
keywords: Coccidiostats; Egg; LC-MS/MS; Poultry; Residues; Validation