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Advisor(s)
Abstract(s)
Pela importância do teor mineral nos vinhos em termos de segurança alimentar e qualidade é imperativo que os laboratórios possuam métodos validados para a sua análise e controlo, garantindo a aplicabilidade do ensaio para implementação em trabalho de rotina. O presente trabalho pretende validar um método de análise multi-elementar por ICP-OES em vinhos, mostos e aguardentes. Estudaram-se parâmetros de validação como seletividade e especificidade, quantificação, limiares analíticos, precisão e exatidão. Validou-se o método para quatro elementos: cálcio, ferro, cobre e potássio. Comprovou-se a especificidade do método pela obtenção de taxas de recuperação próximas de 100%. Verificou-se que as funções de calibração seguem um comportamento linear e calcularam-se os limites de deteção e quantificação, que demonstraram a precisão dos valores reportados na gama de trabalho aplicada. Demonstrou-se que o elemento mais sensível é o ferro e o menos sensível é o potássio. O método revelou-se preciso pela obtenção de coeficientes de variação dentro do limite estipulado e a exatidão foi comprovada através da participação em ensaios laboratoriais com a realização de testes de aptidão.
Due to the importance of mineral content in wines in terms of food safety and quality, it is mandatory that laboratories have validated methods for their analysis and control, guaranteeing the applicability of the test for routine implementation. The present work intends to validate a multi-element analysis method by ICP-OES in wines, musts and spirits. Validation parameters such as selectivity and specificity, quantification, detection and quantification limits, precision and accuracy were studied. The method was validated for four elements: calcium, iron, copper and potassium. The specificity of the method was confirmed by obtaining recovery rates close to 100%. It was verified that the calibration functions follow a linear behavior, and the detection and quantification limits were calculated, which demonstrated the accuracy of the reported values in the applied working range. It was revealed that the most sensitive element is iron and the least sensitive is potassium. The precision of the method was attested by obtaining coefficients of variation within the stipulated limit and the accuracy was proven through participation in interlaboratory tests.
Due to the importance of mineral content in wines in terms of food safety and quality, it is mandatory that laboratories have validated methods for their analysis and control, guaranteeing the applicability of the test for routine implementation. The present work intends to validate a multi-element analysis method by ICP-OES in wines, musts and spirits. Validation parameters such as selectivity and specificity, quantification, detection and quantification limits, precision and accuracy were studied. The method was validated for four elements: calcium, iron, copper and potassium. The specificity of the method was confirmed by obtaining recovery rates close to 100%. It was verified that the calibration functions follow a linear behavior, and the detection and quantification limits were calculated, which demonstrated the accuracy of the reported values in the applied working range. It was revealed that the most sensitive element is iron and the least sensitive is potassium. The precision of the method was attested by obtaining coefficients of variation within the stipulated limit and the accuracy was proven through participation in interlaboratory tests.
Description
Keywords
Vinho ICP-OES Quantificação Análise multi-elementar Validação de método Wine Quantification Multi-elemental analysis Validation of method