Sistemas de screening para detecção de furfural e hidroximetilfurfural e amostras de cachaça por espectroscopia de reflectância difusa
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Data
2016-02-16
Autores
Milani, Maria Izabel [UNESP]
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Editor
Universidade Estadual Paulista (Unesp)
Resumo
Cachaça é a denominação dada à aguardente de cana-de-açúcar produzida no Brasil com teor alcóolico entre 38-48% (v/v). Um dos parâmetros de qualidade determinado neste tipo de amostra é a somatória de furfural e hidroximetilfurfural, com máximo em 5 mg para cada 100 mL de etanol anidro. Essas substâncias, além de conferir sabor desagradável à bebida possuem potencial mutagênico/ carcinogênico. As metodologias de análise geralmente utilizadas para determinação destes analitos se utilizam de técnicas cromatográficas que, além do elevado custo do equipamento e de manutenção, requem operadores capacitados e utilizam solventes orgânicos tóxicos, nocivos à saúde do operador e ao meio ambiente. Sendo assim, em sua maioria, as técnicas cromatográficas são contrárias aos princípios da Química Verde. Dessa maneira, no presente trabalho foi desenvolvida uma nova metodologia para determinação de furfural e hidroximetilfurfural em amostras de cachaça que seja mais rápida, barata e ambientalmente mais amigável que as metodologias cromatográficas usualmente utilizadas, com detecção por espectroscopia de reflectância difusa. O método desenvolvido apresentou duas curvas analíticas, sendo a do furfural AR = 27,117 C1/2 - 0,0271 com R = 0,997 e a do hidroximetilfurfural AR = 15,822 C1/2 - 0,0263 com R = 0,998. Os limites de quantificação obtidos para cada um dos analitos determinados foram de 7,70x10-6 mol L-1 para o furfural e de 1,00x10-5 mol L-1 para o hidroximetilfurfural. Os testes para avaliação de interferência da matriz apresentaram resultados de recuperação entre 89,5 e 108%, concluindo que a matriz não influencia de maneira significativa na determinação dos analitos. A metodologia desenvolvida foi comparada com um método já descrito na literatura, os resultados obtidos foram comparados estatisticamente pelo teste t de Student, os valores de t calculados foram numericamente inferiores que o valor de t tabelado, indicando que não há diferença estatística entre os valores encontrados pelas duas metodologias.
Cachaça is the name given to sugarcane spirits produced in Brazil with alcohol content from 38 to 48% (v/v). One of the quality parameters analyzed is the sum of furfural and hydroxymethylfurfural, with a maximum value of 5 mg per each 100 mL of anhydrous ethanol. These two substances have a mutagenic/carcinogenic power, besides they give a bad flavor to the beverages. The methodologies usually used to determinate the anlytes are chromatographic techniques that, besides the high cost of the equipaments and its maintenance, they need toxic organic solvents that are harmful to operators and the environment. Therefore, chromatographic techniques are mostly against Green Chemistry principles. In this way, the present study aims to develop a new methodology to determinate furfural and hydroxymethylfurfural in cachaça samples that is faster, cheaper and more eco-friendly than the chromatographic methods usually used, with detection by diffuse reflectance spectroscopy. In the method here described, it was obtained two analytical curves; furfural curve is AR = 27.117 C1/2 – 0.0271 with R = 0,997 and hydroxymethylfurfural curve is AR = 15.822 C1/2 – 0.0263 with R = 0,998. Limits of quantification for each analyte were determined as 7.70x10-6 mol L-1 to furfural and 1.00x10-5 mol L-1 to hydroxymethylfurfural. The test to evaluate matrix interference shows a recovery result between 89,5 and 108%, indicating that the matrix does not have a significant interference in analytes determination. The develop methodology was compared against a methodology already described in literature; the results were compared statically by Studant’s t-test, the calculated values for t-test were numerically lower then the table value, indicating that there is no significant statistic difference between values found by both methods.
Cachaça is the name given to sugarcane spirits produced in Brazil with alcohol content from 38 to 48% (v/v). One of the quality parameters analyzed is the sum of furfural and hydroxymethylfurfural, with a maximum value of 5 mg per each 100 mL of anhydrous ethanol. These two substances have a mutagenic/carcinogenic power, besides they give a bad flavor to the beverages. The methodologies usually used to determinate the anlytes are chromatographic techniques that, besides the high cost of the equipaments and its maintenance, they need toxic organic solvents that are harmful to operators and the environment. Therefore, chromatographic techniques are mostly against Green Chemistry principles. In this way, the present study aims to develop a new methodology to determinate furfural and hydroxymethylfurfural in cachaça samples that is faster, cheaper and more eco-friendly than the chromatographic methods usually used, with detection by diffuse reflectance spectroscopy. In the method here described, it was obtained two analytical curves; furfural curve is AR = 27.117 C1/2 – 0.0271 with R = 0,997 and hydroxymethylfurfural curve is AR = 15.822 C1/2 – 0.0263 with R = 0,998. Limits of quantification for each analyte were determined as 7.70x10-6 mol L-1 to furfural and 1.00x10-5 mol L-1 to hydroxymethylfurfural. The test to evaluate matrix interference shows a recovery result between 89,5 and 108%, indicating that the matrix does not have a significant interference in analytes determination. The develop methodology was compared against a methodology already described in literature; the results were compared statically by Studant’s t-test, the calculated values for t-test were numerically lower then the table value, indicating that there is no significant statistic difference between values found by both methods.
Descrição
Palavras-chave
Cachaça, Furfural, Hidroximetilfurfural, Reflectância, Química verde, Hydroxymethylfurfural, Reflectance, Green chemistry