Extração de compostos fenólicos provenientes de folhas de uvaia (Eugenia pyriformis Cambess.) empregando solventes eutéticos profundos (DES)

Orientador: Prof. Dr. Marcos R. MafraCoorientadora: Dra. Fabiane Oliveira FariasDissertação (mestrado) - Universidade Federal do Paraná, Setor de Tecnologia, Programa de Pós-Graduação em Engenharia de Alimentos. Defesa : Curitiba, 09/03/2020Inclui referências: p. 75-85Resumo: A uvaia (Eugenia pyriformis Cambess.) é uma espécie nativa que exibe alto valor nutricional e farmacológico, interligado a presença de compostos antioxidantes. Suas folhas ainda pouco exploradas, podem ser reaproveitadas com o objetivo de gerar co-produtos de alta qualidade com propriedades bioativas de aplicação industrial. O processo de extração sólido-líquido (ESL) é uma operação unitária que possibilita a obtenção de biocompostos por meio da transferência de massa mediante a aplicação de um solvente. O uso de solventes orgânicos gera aspectos negativos oriundos de sua alta toxicidade, emprego de grandes quantidades de solvente e possível degradação da matriz. Os solventes eutéticos profundos (DES) correspondem a uma classe recente de solventes verdes de baixa toxicidade, com elevado potencial de aplicação, principalmente em matrizes de origem vegetal. Nesse sentido, folhas de uvaia foram selecionadas, caracterizadas por meio de análises físico-químicas e submetidas ao processo de extração, variando as condições de tempo, temperatura e proporção (m·v-1) empregando com os DES. Doadores de hidrogênio, água e etanol foram testados a nível de comparação com os DES. Todos os ensaios foram conduzidos em extração do tipo convencional, sendo os melhores resultados, comparados a técnica assistida por ultrassom (UAE). A avaliação dos extratos foi conduzida através das análises de atividade antioxidante, fenólicos totais e flavonoides. O potencial antimicrobiano foi verificado para os melhores DES pelo teste de disco de difusão. Dentre as condições avaliadas, os melhores resultados foram obtidos à 65 °C, com tempo de 150 minutos e proporção 1:30 (m·v-1). Os DES formados a partir de cloreto de colina:ácido lático; cloreto de colina:glicerol e cloreto de colina:1,2 - propanodiol foram selecionados por apresentarem os maiores rendimentos de extração e de atividade antioxidante. Com relação a eficiência de extração o DES formado a partir do ácido lático exibiu maiores quantidades dos fenólicos totais e atividade antioxidante. Para efeito de comparação foi avaliada a extração empregando DES hidrofóbico, formado a partir de mentol e ácido lático, sendo observado que o extrato obtido a partir desse solvente apresenta maior conteúdo de flavonoides totais. Sobre a extração conduzida em UAE, houve um aumento significativo em todas as análises realizadas. O DES formado por cloreto de colina:ácido lático não apresentou diferença significativa entre os tempos de 30 minutos e 90 minutos de extração. Com relação a atividade antimicrobiana, não foi observado halos de inibição significantes para nenhum dos extratos avaliados, indicando que não houve ação antimicrobiana. Palavras-chave: Solventes verdes. Atividade Antioxidante. Atividade Antimicrobiana. Extração Assistida por Ultrassom.Abstract: The uvaia (Eugenia pyriformis Cambess.) is a native plant that shows high nutritional and pharmacological content, linked to the presence of antioxidant compounds. The leaves still unexplored, can be reused to generate co-products with high-quality correlated to the bioactive properties for industrial applications. The solid-liquid extraction (ESL) is a unit operation that makes it possible to obtain biocompounds by the principle of mass transfer employing a solvent. The use of organic solvents produces negative aspects such as high toxicity, requires large amounts of solvent and degradation of the leave compounds. Deep eutectic solvents (DES) correspond to a novel class of green solvents with low toxicity, high potential applications for plants. Uvaia leaves were selected, characterized by physical-chemical analyzes and submitted to the extraction process, varying the conditions of time, temperature, and ratio (m·v-1) using the DES. Donors of hydrogen, water, and ethanol were tested to compare extraction capableness. All tests were conducted in conventional extraction, and the best results were compared to the ultrasound-assisted technique (UAE). The evaluation of the extracts was carried out by the antioxidant activity, total phenolics, and flavonoids analysis. The antimicrobial potential was evaluated for the best DES by the disk diffusion test. Among the conditions appraised, the best results were obtained at 65 ° C, with a time of 150 minutes, and a ratio of 1:30 (g·mL-1). DES formed by choline chloride: lactic acid; choline chloride: glycerol and choline chloride: 1,2 - propanediol were selected due to the highest extraction and antioxidant yields. Regarding extraction performance, DES formed from lactic acid exhibited higher amounts of total phenolics and antioxidant activity. For comparison, extraction was conducted using hydrophobic DES, formed by menthol and lactic acid, and it was observed that the extract obtained from this solvent has a higher content of total flavonoids. About the extraction conducted in the UAE, there was a significant improvement in all analyses performed. The DES formed by choline chloride: lactic acid showed no significant difference between the times of 30 minutes and 90 minutes of extraction. Concerning antimicrobial activity, was notice no significant inhibition halos to any of the extracts evaluated, indicating that there was no antimicrobial action. Keywords: Green solvents. Antioxidant Activity. Antimicrobial Activity. Ultrasound-Assisted Extraction

Extração de compostos fenólicos provenientes de folhas de uvaia (Eugenia pyriformis Cambess.) empregando solventes eutéticos profundos (DES)

Orientador: Prof. Dr. Marcos R. MafraCoorientadora: Dra. Fabiane Oliveira FariasDissertação (mestrado) - Universidade Federal do Paraná, Setor de Tecnologia, Programa de Pós-Graduação em Engenharia de Alimentos. Defesa : Curitiba, 09/03/2020Inclui referências: p. 75-85Resumo: A uvaia (Eugenia pyriformis Cambess.) é uma espécie nativa que exibe alto valor nutricional e farmacológico, interligado a presença de compostos antioxidantes. Suas folhas ainda pouco exploradas, podem ser reaproveitadas com o objetivo de gerar co-produtos de alta qualidade com propriedades bioativas de aplicação industrial. O processo de extração sólido-líquido (ESL) é uma operação unitária que possibilita a obtenção de biocompostos por meio da transferência de massa mediante a aplicação de um solvente. O uso de solventes orgânicos gera aspectos negativos oriundos de sua alta toxicidade, emprego de grandes quantidades de solvente e possível degradação da matriz. Os solventes eutéticos profundos (DES) correspondem a uma classe recente de solventes verdes de baixa toxicidade, com elevado potencial de aplicação, principalmente em matrizes de origem vegetal. Nesse sentido, folhas de uvaia foram selecionadas, caracterizadas por meio de análises físico-químicas e submetidas ao processo de extração, variando as condições de tempo, temperatura e proporção (m·v-1) empregando com os DES. Doadores de hidrogênio, água e etanol foram testados a nível de comparação com os DES. Todos os ensaios foram conduzidos em extração do tipo convencional, sendo os melhores resultados, comparados a técnica assistida por ultrassom (UAE). A avaliação dos extratos foi conduzida através das análises de atividade antioxidante, fenólicos totais e flavonoides. O potencial antimicrobiano foi verificado para os melhores DES pelo teste de disco de difusão. Dentre as condições avaliadas, os melhores resultados foram obtidos à 65 °C, com tempo de 150 minutos e proporção 1:30 (m·v-1). Os DES formados a partir de cloreto de colina:ácido lático; cloreto de colina:glicerol e cloreto de colina:1,2 - propanodiol foram selecionados por apresentarem os maiores rendimentos de extração e de atividade antioxidante. Com relação a eficiência de extração o DES formado a partir do ácido lático exibiu maiores quantidades dos fenólicos totais e atividade antioxidante. Para efeito de comparação foi avaliada a extração empregando DES hidrofóbico, formado a partir de mentol e ácido lático, sendo observado que o extrato obtido a partir desse solvente apresenta maior conteúdo de flavonoides totais. Sobre a extração conduzida em UAE, houve um aumento significativo em todas as análises realizadas. O DES formado por cloreto de colina:ácido lático não apresentou diferença significativa entre os tempos de 30 minutos e 90 minutos de extração. Com relação a atividade antimicrobiana, não foi observado halos de inibição significantes para nenhum dos extratos avaliados, indicando que não houve ação antimicrobiana. Palavras-chave: Solventes verdes. Atividade Antioxidante. Atividade Antimicrobiana. Extração Assistida por Ultrassom.Abstract: The uvaia (Eugenia pyriformis Cambess.) is a native plant that shows high nutritional and pharmacological content, linked to the presence of antioxidant compounds. The leaves still unexplored, can be reused to generate co-products with high-quality correlated to the bioactive properties for industrial applications. The solid-liquid extraction (ESL) is a unit operation that makes it possible to obtain biocompounds by the principle of mass transfer employing a solvent. The use of organic solvents produces negative aspects such as high toxicity, requires large amounts of solvent and degradation of the leave compounds. Deep eutectic solvents (DES) correspond to a novel class of green solvents with low toxicity, high potential applications for plants. Uvaia leaves were selected, characterized by physical-chemical analyzes and submitted to the extraction process, varying the conditions of time, temperature, and ratio (m·v-1) using the DES. Donors of hydrogen, water, and ethanol were tested to compare extraction capableness. All tests were conducted in conventional extraction, and the best results were compared to the ultrasound-assisted technique (UAE). The evaluation of the extracts was carried out by the antioxidant activity, total phenolics, and flavonoids analysis. The antimicrobial potential was evaluated for the best DES by the disk diffusion test. Among the conditions appraised, the best results were obtained at 65 ° C, with a time of 150 minutes, and a ratio of 1:30 (g·mL-1). DES formed by choline chloride: lactic acid; choline chloride: glycerol and choline chloride: 1,2 - propanediol were selected due to the highest extraction and antioxidant yields. Regarding extraction performance, DES formed from lactic acid exhibited higher amounts of total phenolics and antioxidant activity. For comparison, extraction was conducted using hydrophobic DES, formed by menthol and lactic acid, and it was observed that the extract obtained from this solvent has a higher content of total flavonoids. About the extraction conducted in the UAE, there was a significant improvement in all analyses performed. The DES formed by choline chloride: lactic acid showed no significant difference between the times of 30 minutes and 90 minutes of extraction. Concerning antimicrobial activity, was notice no significant inhibition halos to any of the extracts evaluated, indicating that there was no antimicrobial action. Keywords: Green solvents. Antioxidant Activity. Antimicrobial Activity. Ultrasound-Assisted Extraction

Valorization of Raw Coffee Beans (<i>Coffea arabica</i> and <i>Coffea canephora</i>) through Solvent Development and Extraction of Bioactive Compounds

Raw coffee beans are seen as valuable sources of bioactive compounds, such as alkaloids and chlorogenic acids. In this study, an efficient and eco-friendly method for the simultaneous extraction of caffeine, trigonelline, and chlorogenic acids from raw beans of two coffee species was developed, using green solvents and an unconventional method of extraction (assisted by ultrafast rotary disintegrator/homogenizer (UT-AE)). The experimental extraction conditions were optimized according to a completely randomized design (CRD), considering the following variables: solvent type (four deep eutectic solvents (DESs), water, and aqueous choline chloride solution (50 wt.%); temperature (25, 45, and 65 °C); and extraction technique (solid-liquid extraction with agitated heating and assisted by ultrafast rotary disintegrator/homogenizer). The extract obtained with choline chloride solution (50 wt.%) exhibited high total phenolic compounds and the highest antioxidant capacity. An analysis using high-performance liquid chromatography with a diode array detector (HPLC-DAD) indicated the presence of chlorogenic acids, caffeine, and trigonelline in all the extracts, in different amounts. The results obtained by the analysis of phenolic compounds and HPLC indicated that the aqueous solution of choline chloride (50% wt.%) was the most suitable solvent for the extraction of chlorogenic acids, while the water-based extracts showed high values of caffeine and trigonelline. DESs, in turn, seems to promote a protective effect on the antioxidant activity of biomolecules

Valorization of Raw Coffee Beans (Coffea arabica and Coffea canephora) through Solvent Development and Extraction of Bioactive Compounds

Raw coffee beans are seen as valuable sources of bioactive compounds, such as alkaloids and chlorogenic acids. In this study, an efficient and eco-friendly method for the simultaneous extraction of caffeine, trigonelline, and chlorogenic acids from raw beans of two coffee species was developed, using green solvents and an unconventional method of extraction (assisted by ultrafast rotary disintegrator/homogenizer (UT-AE)). The experimental extraction conditions were optimized according to a completely randomized design (CRD), considering the following variables: solvent type (four deep eutectic solvents (DESs), water, and aqueous choline chloride solution (50 wt.%); temperature (25, 45, and 65 &deg;C); and extraction technique (solid-liquid extraction with agitated heating and assisted by ultrafast rotary disintegrator/homogenizer). The extract obtained with choline chloride solution (50 wt.%) exhibited high total phenolic compounds and the highest antioxidant capacity. An analysis using high-performance liquid chromatography with a diode array detector (HPLC-DAD) indicated the presence of chlorogenic acids, caffeine, and trigonelline in all the extracts, in different amounts. The results obtained by the analysis of phenolic compounds and HPLC indicated that the aqueous solution of choline chloride (50% wt.%) was the most suitable solvent for the extraction of chlorogenic acids, while the water-based extracts showed high values of caffeine and trigonelline. DESs, in turn, seems to promote a protective effect on the antioxidant activity of biomolecules

Empagliflozin in Patients with Chronic Kidney Disease

Background The effects of empagliflozin in patients with chronic kidney disease who are at risk for disease progression are not well understood. The EMPA-KIDNEY trial was designed to assess the effects of treatment with empagliflozin in a broad range of such patients. Methods We enrolled patients with chronic kidney disease who had an estimated glomerular filtration rate (eGFR) of at least 20 but less than 45 ml per minute per 1.73 m(2) of body-surface area, or who had an eGFR of at least 45 but less than 90 ml per minute per 1.73 m(2) with a urinary albumin-to-creatinine ratio (with albumin measured in milligrams and creatinine measured in grams) of at least 200. Patients were randomly assigned to receive empagliflozin (10 mg once daily) or matching placebo. The primary outcome was a composite of progression of kidney disease (defined as end-stage kidney disease, a sustained decrease in eGFR to &lt; 10 ml per minute per 1.73 m(2), a sustained decrease in eGFR of &amp; GE;40% from baseline, or death from renal causes) or death from cardiovascular causes. Results A total of 6609 patients underwent randomization. During a median of 2.0 years of follow-up, progression of kidney disease or death from cardiovascular causes occurred in 432 of 3304 patients (13.1%) in the empagliflozin group and in 558 of 3305 patients (16.9%) in the placebo group (hazard ratio, 0.72; 95% confidence interval [CI], 0.64 to 0.82; P &lt; 0.001). Results were consistent among patients with or without diabetes and across subgroups defined according to eGFR ranges. The rate of hospitalization from any cause was lower in the empagliflozin group than in the placebo group (hazard ratio, 0.86; 95% CI, 0.78 to 0.95; P=0.003), but there were no significant between-group differences with respect to the composite outcome of hospitalization for heart failure or death from cardiovascular causes (which occurred in 4.0% in the empagliflozin group and 4.6% in the placebo group) or death from any cause (in 4.5% and 5.1%, respectively). The rates of serious adverse events were similar in the two groups. Conclusions Among a wide range of patients with chronic kidney disease who were at risk for disease progression, empagliflozin therapy led to a lower risk of progression of kidney disease or death from cardiovascular causes than placebo