Desenvolvimento de método robusto, eficiente e de baixo impacto ambiental para se obter perfil cromatográfico de vinhos brasileiros por CLAE
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Data
2019-03-01
Autores
Pelissari, João Henrique [UNESP]
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Editor
Universidade Estadual Paulista (Unesp)
Resumo
Diversos métodos já foram desenvolvidos para a identificação de compostos fenólicos em vinhos, contudo, tais métodos utilizam solventes tóxicos que podem prejudicar desde o meio ambiente até a saúde do analista. Diante disso, este trabalho descreve o desenvolvimento racional e eficiente de um método por cromatografia líquida de alta eficiência capaz de identificar os principais constituintes químicos em amostras dos vinhos brasileiros merlot e cabernet suavignon, abordando os princípios da Química Analítica Verde. Para o desenvolvimento do método foi utilizado como solvente orgânico da fase móvel o etanol, solvente biodegradável e sustentável. Como etapa inicial foi utilizado um planejamento fatorial fracionário de dois níveis com 7 fatores (2V7-2), do qual foi possível observar que a temperatura e a porcentagem inicial de etanol foram os parâmetros cromatográficos que mais influenciaram na separação dos compostos fenólicos. Após a identificação dos fatores mais influentes, os mesmos foram submetidos a um planejamento Doehlert para a obtenção da melhor condição cromatográfica. O método cromatográfico desenvolvido foi eficiente na separação dos principais constituintes dos vinhos, possibilitando a identificação de: ácido gálico, ácido cafeico, ácido siríngico, ácido p-cumárico, resveratrol, kaempferol, catequina e epicatequina. O método também apresentou precisão na faixa de 0,19 a 0,95%, considerada adequada segundo os critérios estabelecidos pela ANVISA. Além disso, foi determinado a impacto ambiental utilizando a métrica HPLC-EAT da qual foi possível obter uma pontuação de 20,114, classificando o método como verde quando comparado com os da literatura, os quais obtiveram pontuações que variaram de 28,545 a 125,610. O método desenvolvido contemplou 8 princípios dos 12 da Química Analítica Verde.
Several methods have already been developed for the identification of phenolic compounds in wines. However, such methods employ toxic solvents that can harm from the environment to the health of the analyst. At that, this work describes the rational and efficient development of a High Performance Liquid Chromatography method capable of identify the main chemical constituents in samples of brazilian wines merlot and cabernet sauvignon, approaching the principles of Green Analytical Chemistry. To the development of the method, ethanol was used as the organic solvent for the mobile phase, a biodegradable and sustainable solvent. A fractional factorial design with 2 levels and 7 factors (2V7-2) was used as the initial step, from which it was possible to observe that the temperature and the initial percentage of ethanol were the chromatographic parameters that most influenced in the separation of the phenolic compounds. Once the most important factors were identified, they were submitted to Doehlert design to obtain the best chromatographic condition. The chromatographic method developed was efficient in separating the main constituents of the wines, allowing the identification of: gallic acid, caffeic acid, syringic acid, p-coumaric acid, resveratrol, kaempferol, catechin and epicatechin. The method also presented precision in the range of 0.19 to 0.95%, considered adequate according to the criteria established by ANVISA. In addition, the environmental impact was determined using the HPLC-EAT metric from which it was possible to obtain a score of 20.114, classifying the method as green when compared to the literature, which obtained scores that ranged from 28.545 to 125.610. The method developed contemplated 8 principles of the 12 of the Green Analytical Chemistry.
Several methods have already been developed for the identification of phenolic compounds in wines. However, such methods employ toxic solvents that can harm from the environment to the health of the analyst. At that, this work describes the rational and efficient development of a High Performance Liquid Chromatography method capable of identify the main chemical constituents in samples of brazilian wines merlot and cabernet sauvignon, approaching the principles of Green Analytical Chemistry. To the development of the method, ethanol was used as the organic solvent for the mobile phase, a biodegradable and sustainable solvent. A fractional factorial design with 2 levels and 7 factors (2V7-2) was used as the initial step, from which it was possible to observe that the temperature and the initial percentage of ethanol were the chromatographic parameters that most influenced in the separation of the phenolic compounds. Once the most important factors were identified, they were submitted to Doehlert design to obtain the best chromatographic condition. The chromatographic method developed was efficient in separating the main constituents of the wines, allowing the identification of: gallic acid, caffeic acid, syringic acid, p-coumaric acid, resveratrol, kaempferol, catechin and epicatechin. The method also presented precision in the range of 0.19 to 0.95%, considered adequate according to the criteria established by ANVISA. In addition, the environmental impact was determined using the HPLC-EAT metric from which it was possible to obtain a score of 20.114, classifying the method as green when compared to the literature, which obtained scores that ranged from 28.545 to 125.610. The method developed contemplated 8 principles of the 12 of the Green Analytical Chemistry.
Descrição
Palavras-chave
Vinho, Cromatografia líquida de alta eficiência, Quimiometria, Química verde, Planejamento experimental