Resíduos de agrotóxicos em feijão (Phaseolus vulgaris L.): validação de método, ocorrência no Brasil, organização de ensaio de proficiência e produção de material de referência certificado.

• Ano de defesa: 2016
• Autor(a) principal: Márcia Cassimira Marcos Ribeiro
• Tipo de documento: Tese
• Tipo de acesso: Acesso aberto
• Idioma: por
• Instituição de defesa: Universidade Federal de Minas Gerais; Brasil; FARMACIA - FACULDADE DE FARMACIA; Programa de Pós-Graduação em Ciência de Alimentos; UFMG
• Palavras-chave em Português: Garantia da qualidade analítica; Avaliação externa da qualidade; Rastreabilidade metrológica; Controle de alimentos
• Link de acesso: http://hdl.handle.net/1843/35042

A method for analysis of multiresidues of pesticides in common beans (Phaseolus vulgaris L.) was developed and validated. The extraction and purification were carried out by a modified QuEChERS method and the detection and quantification were reached by liquid chromatography tandem triple quadrupole mass spectrometer. The method was fit for the purpose of quantification of 112 pesticides. The occurrence of pesticide residues in commercial beans was studied with the validated method in 256 samples collected in all Brazilian states and the Federal District. A proficiency test with thirteen laboratories was also conducted for the analysis of eight pesticides in organic common beans. The proficiency test items were homogeneous and stable during the test period. The results of the participants were evaluated by three different proficiency methods: Algorithm A of ISO 13.528: 2015, median with normalized interquartile range and consistency factors k and h of ISO 5725-2:1994. The results demonstrated that the method of ISO 5725-25725-2: 1994 was more appropriate for the data analysis. The laboratories that analyzed all the pesticide residues and obtained all satisfactory results in the proficiency test were selected for the characterization of a candidate reference material containing twelve pesticides added to organic beans. After evaluation of the homogeneity, the stability to the transport and the long term stability, and the characterization of the candidate reference material, the certified values and their respective uncertainties were: 0.061 mg/kg ± 0.011 mg/kg for acetamiprid; 0.082 mg/kg ± 0.037 mg/kg for cyproconazole; 0.065 mg/kg ± 0.018 mg/kg for flutriafol; 0.072 mg/kg ± 0.013 mg/kg for imidacloprid; 0.048 ± 0.022 mg/kg for pyraclostrobin; 0.049 mg/kg ± 0.023 mg/kg for pyriproxyfen; and 0.079 mg/kg ± 0.009 mg/kg for propiconazole