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Implementação do método de análise de adoçantes não calóricos em matrizes alimentares por cromatografia líquida de alta eficiência (HPLC-UV)
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Abstract(s)
Este trabalho foi elaborado na Silliker Portugal, S.A. com o objetivo de implementar e validar um novo método para a determinação de acessulfame K, aspartame e sacarina, em matrizes alimentares utilizando HPLC-UV. Para o estudo foram ensaiadas várias matrizes, vinho, gelatina, adoçante em pó e líquido de stevia, barra energética, iogurte, leite e ice tea. Para a validação da metodologia foram estudados a precisão, exatidão, justeza e
linearidade. Para o estudo da precisão determinaram-se limites de repetibilidade abaixo dos 14% e limites de precisão intermédia inferiores a 10%. Para a exatidão foi utilizado um material de referência FAPAS e todos os ensaios realizados apresentaram um z-score inferior a 2. Quanto à justeza, efetuaram-se ensaios de recuperação cujos resultados se situaram entre 80% e 120%. Confirmou-se também que existe linearidade entre 2 e 100
mg/l. Após a análise destes resultados concluiu-se que o método cumpre com os requisitos necessários de precisão e de exatidão. Paralelamente foi também efetuado um estudo sobre os efeitos da refrigeração ao longo
do tempo, na leitura dos padrões analíticos, e concluiu-se que para a sacarina e aspartame existe estabilidade das soluções, enquanto que para o acessulfame o mesmo estudo foi inconclusivo.
This work was developed at Silliker Portugal, S.A with the objective of implementing and validating a new method for the determination of acessulfame K, aspartame and saccharin, in multiple matrices using HPLC-UV. For the study, several matrices were evaluated: wine, gelatin, powdered and liquid stevia sweetener, energy bar, yogurt, milk and iced tea. To validate the methodology, precision, accuracy, fairness, and linearity were studied. For the precision study, repeatability limits of less than 14% and intermediate precision limits of less than 10% were determined. For accuracy, a FAPAS reference material was used, and all assays performed presented a z-score below 2. For fairness, recovery tests were performed, with results ranging from 80 % to 120%. Linearity was also observed between 2 and 100 mg/L. After analyzing these results, it was concluded that the method meets the necessary precision and accuracy requirements. At the same time, a study was also carried out on the effects of refrigeration over time, on the reading of analytical standards, and it was concluded that for saccharin and aspartame there is stability in the solutions, while for acesulfame the same study was inconclusive.
This work was developed at Silliker Portugal, S.A with the objective of implementing and validating a new method for the determination of acessulfame K, aspartame and saccharin, in multiple matrices using HPLC-UV. For the study, several matrices were evaluated: wine, gelatin, powdered and liquid stevia sweetener, energy bar, yogurt, milk and iced tea. To validate the methodology, precision, accuracy, fairness, and linearity were studied. For the precision study, repeatability limits of less than 14% and intermediate precision limits of less than 10% were determined. For accuracy, a FAPAS reference material was used, and all assays performed presented a z-score below 2. For fairness, recovery tests were performed, with results ranging from 80 % to 120%. Linearity was also observed between 2 and 100 mg/L. After analyzing these results, it was concluded that the method meets the necessary precision and accuracy requirements. At the same time, a study was also carried out on the effects of refrigeration over time, on the reading of analytical standards, and it was concluded that for saccharin and aspartame there is stability in the solutions, while for acesulfame the same study was inconclusive.
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Keywords
Segurança Alimentar Adoçantes Implementação de método de análise Validação de método de análise HPLC Food safety Sweeteners Analysis method implementation Analysis method validation