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Determinação dos Teores de Acrilamida em alimentos por Cromatografia Líquida de Ultra Eficiência
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Este trabalho tem por objetivo principal validar o método analítico de quantificação dos
níveis de acrilamida em alimentos por cromatografia líquida de ultra eficiência acoplada à es-
pectrometria de massa em tandem (UPLC-MS/MS), com ionização por electrospray.
Foram analisadas as matrizes alimentares mais comumente analisadas no laboratório
da SGS e que possuíam um maior teor de acrilamida através de diversos métodos de extração,
até concluir o que melhor se adequava às condições laboratoriais de modo a alcançar os resul-
tados pretendidos para a validação do mesmo. As três matrizes alimentares validadas são pão,
batatas fritas e bolachas/cereais, e o analito de interesse é extraído a partir dos alimentos pão e
bolachas/cereais através de uma solução aquosa de ácido acético e das soluções Carrez I e II e
por extração em fase sólida no caso da matriz da batata frita e bolachas/cereais, devido à sua
complexidade matricial.
Está comprovado que o consumo de acrilamida potencia o risco de desenvolvimento de
cancro. É considerada um contaminante pela Comissão da União Europeia implementou me-
didas de mitigação e níveis de referência, o que leva a um controlo de qualidade rigoroso em
certos grupos alimentares específicos de modo a proteger a saúde dos consumidores e regular
os seus níveis nos respetivos alimentos.
Para a validação do método analítico por cada tipo de matriz foram avaliados os parâ-
metros da especificidade e seletividade, das curvas de calibração bem como o estudo sobre a
sua linearidade, da precisão com um estudo da reprodutibilidade e precisão intermédia, dos
limites analíticos, da robustez e da exatidão.
Verifica-se após a avaliação dos parâmetros para a validação do método analítico de
cada uma das matrizes, que estes são aceites pelos critérios estabelecidos e, por tanto, o objetivo
proposto foi atingido e os métodos analíticos podem ser aplicados na rotina diária do laboratório da SGS.
The main objective of this work is to validate the analytical method for quantifying acrylamide levels in foods by ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS), with electrospray ionization. The food matrixes most commonly analyzed in the SGS laboratory and that had the highest acrylamide content were analyzed using several extraction methods, until the one that best suited the laboratory conditions was concluded in order to achieve the desired results for its validation. The three food matrices validated are bread, potato French fries and crackers/ce- reals, and the analyte of interest is extracted from the bread and crackers/cereals foods through an aqueous solution of acetic acid and Carrez I and II solutions and by solid phase extraction in the case of the potato chips and crackers/cereals matrix due to its matrix complexity. It has been proven that the consumption of acrylamide increases the risk of developing cancer. It is considered a contaminant by the European Commission and has implemented mit- igation measures and reference levels, which leads to strict quality control in certain specific food groups in order to protect consumers health and regulate its levels in their food. For the validation of the analytical method for each type of matrix, the parameters of specificity and selectivity, the calibration curves were evaluated as well as the study on their linearity, precision with a study on reproducibility and intermediate precision, analytical limits, robustness and accuracy. After the evaluation of the parameters for the validation of the analytical method for each of the matrixes, it is verified that they are accepted by the established criteria and, there- fore, the proposed objective was achieved, and the analytical methods can be applied in the daily routine of the SGS laboratory.
The main objective of this work is to validate the analytical method for quantifying acrylamide levels in foods by ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS), with electrospray ionization. The food matrixes most commonly analyzed in the SGS laboratory and that had the highest acrylamide content were analyzed using several extraction methods, until the one that best suited the laboratory conditions was concluded in order to achieve the desired results for its validation. The three food matrices validated are bread, potato French fries and crackers/ce- reals, and the analyte of interest is extracted from the bread and crackers/cereals foods through an aqueous solution of acetic acid and Carrez I and II solutions and by solid phase extraction in the case of the potato chips and crackers/cereals matrix due to its matrix complexity. It has been proven that the consumption of acrylamide increases the risk of developing cancer. It is considered a contaminant by the European Commission and has implemented mit- igation measures and reference levels, which leads to strict quality control in certain specific food groups in order to protect consumers health and regulate its levels in their food. For the validation of the analytical method for each type of matrix, the parameters of specificity and selectivity, the calibration curves were evaluated as well as the study on their linearity, precision with a study on reproducibility and intermediate precision, analytical limits, robustness and accuracy. After the evaluation of the parameters for the validation of the analytical method for each of the matrixes, it is verified that they are accepted by the established criteria and, there- fore, the proposed objective was achieved, and the analytical methods can be applied in the daily routine of the SGS laboratory.
Descrição
Palavras-chave
Acrilamida UPLC-MS/MS Implementação Validação Matrizes Alimentares Extração por Solventes