Evalueringsgruppens vurderinger

No presente trabalho desenvolveu-se uma metodologia de análise por injeção sequencial (SIA) que permite quantificar a melamina em amostras alimentares lácteas e, portanto, controlar se o seu teor se encontra abaixo dos 2,5 mg/L (ppm), valor máximo de melamina admitida em produtos lácteos na União Europeia.

Relativamente às metodologias já existentes, verifica-se que a metodologia SIA desenvolvida apresenta valores de limite superior de resposta linear (2,58 mg/L) e de limite de deteção (0,12 mg/L) que se enquadram na gama de valores apresentadas nesses trabalhos. É ainda de realçar o bom índice de percentagem de recuperação face a algumas metodologias e, a vantagem única de não apresentar pré-tratamento de amostra/processo de extração fora do sistema, etapas que habitualmente são morosas e sujeitas a menor repetibilidade devido a erros operacionais. [125]

Com o sistema de fluxo proposto é possível, simultaneamente, a extração automática da melamina, e a sua determinação. Para isso incorporou-se na montagem uma unidade de extração com membrana hidrofílica, através da qual as amostras alimentares lácteas eram inseridas sem qualquer tipo de pré-tratamento ou intervenção do operador. A posterior determinação da melamina no sistema de fluxo foi efetuada com base na reação de oxidação do sesamol pelo peróxido de hidrogénio, catalisada pela peroxidase e na presença de líquido iónico.

A metodologia desenvolvida é automática e económica, incorporando equipamentos relativamente simples, permite cerca de 11 determinações por hora de forma reprodutível, com consumo reduzido de reagentes e baixa produção de efluentes. A introdução do líquido iónico, em substituição de outros componentes orgânicos tradicionais para a etapa da extração, permitiu tornar esta metodologia ainda mais integrada na “Química verde” e sustentável quanto aos efluentes.

O estudo de interferências, assim como de variação de pH das amostras, permite concluir sobre a robustez da metodologia quando na presença de possíveis elementos que naturalmente constituem as amostras alimentares lácteas.

Adicionalmente, os diferentes ensaios de recuperação (89,3-110,4%) efetuados, em diversas amostras, confirmam a aplicabilidade da metodologia a este tipo de matriz.

Esta aplicação analítica permitiu confirmar a versatilidade e robustez da técnica SIA. A utilização da válvula multiposições, como elemento central, e o modo de funcionamento baseado em inversões do sentido de fluxo, a partir da válvula, permitiu não só a incorporação de diversos dispositivos como facilitou a gestão e direcionamento

70 de amostra e reagentes, abrindo inúmeras possibilidades em termos de manipulação de amostra e deteção do produto final.

Com todos os estudos efetuados pode, assim, considerar-se que metodologia desenvolvida apresenta condições para integrar um laboratório de controlo de qualidade, permitindo efetuar, com robustez e agilidade, análises ao parâmetro melamina, assegurando assim que as amostras se encontram abaixo dos limites legais em vigor.

71

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