Otimização e validação de método para determinação de histamina em pescado

• Ano de defesa: 2008
• Autor(a) principal: Tarliane Maria da Silva
• Tipo de documento: Dissertação
• Tipo de acesso: Acesso aberto
• Idioma: por
• Instituição de defesa: Universidade Federal de Minas Gerais; UFMG
• Palavras-chave em Português: CLAE; qualidade; Peixe; método analítico; histamina; Cromatografia líquida de alta eficiência; Alimentos Contaminação; Pescados Análise; Pescados Contaminação; Histamina
• Link de acesso: http://hdl.handle.net/1843/URMR-7RYPJ5

The exportation of fresh fish to Europe has been limited by therequirement of certificates with the levels of histamine. The method recommended for the analysis is high performance liquid hromatography (HPLC). Histamine is extracted with perchloric acid and derivatized prior to analysis. However, the extractor is explosive and the derivatization reaction requires excessive handling which can affectnegatively the efficiency of the method. Furthermore, since the analysis takes a long time, the exportation of fresh fish is limited. In order to solve such problems, the objective of this work was to optimize and validate an efficient and rapid HPLC method for the determination of histamine in fish. The extraction was optimized and the defined parameters were sample homogenization for 70 s; 11250 x g, 3 min and 0 C for thespeed, time and temperature of centrifugation, respectively. Under these conditions, the extraction time was reduced from 90 to 15 minutes, compared to the recommended method. The internal standard (1,3-diaminopropane) recomended by DUFLOS et al. (1999), co-eluted with phenylethylamine and putrescine, and, therefore, could not beused. Comparing the analytical procedures used by DUFLOS et al. (1999) and adapted from VALE & GLORIA (1997), the last one was the most appropriate for the analysis of histamine in fish, and it was chosen for further studies. The method was optimized and validated: it was linear in the range of 0.2 to 60 Êg/mL; there was no effect of the matrix;and the method was selective, exact and precise. The method was considered viable for the analysis of histamine in fish as recommended by the Europeian Union which requires limits of 100 to 200 mg/kg. Furthermore, it could be performed in a shorter period of time compared to the original method. Using this method, the levels of histamine were determined in fresh and canned tuna samples commercialized in /beloHorizonte, state of Minas Gerais, Brazil. Every sample analyzed was in compliance with the Mercosur, FDA and Europeian Union standards.