DESENVOLVIMENTO DE METODOLOGIA PARA ANÁLISE DE SULFONAMIDAS EM MEL UTILIZANDO CROMATOGRAFIA LÍQUIDA E DETECÇÃO POR ARRANJO DE DIODOS / DEVELOPMENT OF METHODOLOGY FOR ANALYSIS SULFONAMIDES IN HONEY USING LIQUID CHROMATOGRAPHY AND DETECTION DIODE ARRAY
AUTOR(ES)
VERÔNICA ALVES GONÇALVES DA SILVA
DATA DE PUBLICAÇÃO
2008
RESUMO
Honey is a natural substance produced by bees and by your nature it is considered a healthy product. Presence of additives and/or preserve agents is not permitted. On apiculture, sulfonamydes are largely used on prevention and control of beehive disease, such as American foulbrood caused by Paenibacillus larvae. A consequence of this practice is the presence of these residues in honey, that should cause allergy reactions on consumers. In the last years, some publicated works is discussing the presence of antibiotic and sulfonamides residues in honey. In Brazil, the presence of antibiotics residues in food is controled by the Agência Nacional de Vigilância Sanitária (ANVISA) an by the Ministério da Agricultura, Pecuária e do Abastecimento (MAPA). The realization of monitoring contaminants residues in food programs, as well as the Plano Nacional de Controle de Resíduos (PNCR) from MAPA are essentials to the sanitary vigilance actions development, preventing and controlling possible hazard to the consumer health. This work has the objective the development and validation of multiresidue analytical method to the sulfadiazine, sulfathiazole, sulfadimedine and sulfadimethoxine determination in bee honey using high performance liquid chromatography (HPLC) with diode array detector (DAD). The established methodology consisted on such conditions: solid phase extraction with Nexus sorbent, elution with acetonitrile 5 mL, and reconstitution with sodium acetate buffer (0,05 mol L-1) pH 4,5, with 1% methanol addition, separation on analytical column C18, acetonitrile and water mobile phase, on gradient elution mode and detection on 278 nm. The sample preparation consisted on the acid hydrolysis with hydrochloric acid 2 mol L-1 of a honey rate and adjust to pH 4,5 with sodium acetate buffer solution 0,05 mol L-1 pH 4,5. The method was validated and the results demonstrated accuracy and precision between the limits established by the current legislation. Good linearity range was encountered, obtaining recovery values varying from 41 to 89% and relative standard deviation estimative varying between 2,36 and 14% to the four studied compounds. The four sulfonamides detection limits in honey sample varying from 20 to 30 ^g kg-1 and the quantification limits varied from 60 to 90 ^g kg-1. Considering 100 ^g kg-1 the residue maximum limit established by the Brazilian legislation to the SDZ, STZ, SMZ and SDM total concentration, the described method permit suitable determination of the four sulfonamides in bee honey.
ASSUNTO(S)
sulfonamidas validação honey quimica analitica clae-dad hplc-dad extração por fase sólida validation mel solid phase extraction
ACESSO AO ARTIGO
http://www.tedebc.ufma.br//tde_busca/arquivo.php?codArquivo=460Documentos Relacionados
- DESENVOLVIMENTO DE MÉTODO MULTIRESIDUAL PARA ANÁLISE DE PESTICIDAS EM MEL, UTILIZANDO CROMATOGRAFIA A LÍQUÍDO COM DETECTOR ESPECTROFOTOMÉTRICO COM ARRANJO DE DIODOS
- Development of analyrtical methods for determination of N-nitrosamines in shampoo samples by liquid chromatography coupled to diode array, electrochemical and mass spectrometry detecto
- Desenvolvimento e validação de metodologia para análise simultânea de aminoácidos como possíveis marcadores neurobiológicos da esquizofrenia utilizando a cromatografia líquida de alta eficiência com detecção por fluorescência
- DEVELOPMENT AND VALIDATION OF METHODOLOGY FOR THE EVALUATION OF RUPATADINE BY LIQUID CHROMATOGRAPHY AND CAPILLARY ELECTROPHORESIS
- DEVELOPMENT AND VALIDATION OF METHODOLOGY FOR THE EVALUATION OF FLUTICASONE BY LIQUID CHROMATOGRAPHY AND CAPILLARY ELECTROPHORESIS