Supercritical fluids and fluid mixtures to obtain high-value compounds from Capsicum peppers

Peppers of the Capsicum genus have a rich nutritional composition and are widely consumed worldwide. Thus, they find numerous applications in the food, pharmaceutical and cosmetic industries. One commercial application is oleoresin production, a nonpolar fraction rich in bioactive compounds, including capsaicinoids and carotenoids. Among the technologies for pepper processing, special attention is given to supercritical fluid technologies, such as supercritical fluid extraction (SFE) with pure solvents and CO2 plus modifiers, and SFE assisted by ultrasound. Supercritical fluid-based processes present advantages over the classical extraction techniques like using less solvents, short extraction times, specificity and scalability. In this review, we present a brief overview of the nutritional aspects of peppers, followed by studies that apply supercritical fluid technologies to produce extracts and concentrate bioactives, besides oleoresin encapsulation. Furthermore, we present related phase equilibrium, cost estimation, and the gaps and needs for the full use of peppers from a sustainable perspective

Combining eutectic solvents and pressurized liquid extraction coupled in-line with solid-phase extraction to recover, purify and stabilize anthocyanins from Brazilian berry waste

Pressurized techniques are straightforward for high-scale applications and highly controllable, which seems an excellent strategy for recovering unstable natural compounds. In this work, the main advance was the development of a platform based on the pressurized liquid extraction coupled in-line with a solid-phase extraction step (PLE-SPE) combined with the use of eutectic mixtures as solvents to promote an efficient extraction and purification of natural pigments from food wastes. Eutectic mixtures, conventionally known as (deep) eutectic solvents – (D)ES, are combinations of two or more substances with a lower melting point than any of their components. (D)ES are often referred as “green solvents” because they can potentially be more environmentally friendly than other solvents, especially volatile organic solvents (VOSs). Overall, (D)ES have the potential to contribute to the achievement of several of the SDGs (especially 3, 13, and 14) through their positive impacts on health, environment, and sustainable production and consumption practices. Thus, in this work, (D)ES were used as solvents to valorize Brazilian berry waste (Plinia cauliflora). Anthocyanins are the biomass's main compounds of commercial interest, mainly for food and cosmetic applications. However, there are several technological issues regarding color control due to their high sensitivity to light, heat, oxygen, and pH variations. Thus, the data achieved in this work highlighted the high efficiency and low environmental footprint of the PLE-SPE-(D)ES platform developed. The success of the downstream process here developed was proved by the high extraction efficiency and the purity level of the anthocyanins obtained. Besides, thermal stability analysis was evaluated, demonstrating that (D)ES are not only solvents but also stabilizing agents, improving the shelf-life of the extracted colorants.publishe

Potential application for antimicrobial and antileukemic therapy of a flavonoid-rich fraction of Camellia sinensis

The antimicrobial and antileukemic effect of a purified fraction of flavonoids from the leaves of Camellia sinensis was evaluated. An extraction yield of 9.77 mg.g-1 total flavonoids was recovered through a pressurized liquid extraction associated with solid-phase extraction. This fraction was tested against pathogenic microorganisms (Staphylococcus, Salmonella, and Enterococcus), considering the minimum inhibitory concentration. In addition, the human monocyte cell line THP-1, derived from a patient with acute monocytic leukemia, was used for the antitumor assay. The results show that the flavonoid-rich fraction obtained by coupling a Pressurized Liquids Extraction in-line with a Solid Phase Extraction (PLE-SPE) has a high antimicrobial effect and resulted in cell cycle blockage G0 / G1, increased DNA fragmentation, and altered leukemic cell morphology. These results suggest that a flavonoid-rich fraction obtained from Camellia sinensis can be applied as potential adjuvants in chemotherapy treatment to mitigate the side effects caused by chemotherapy or even as a supplement to cancer therapy9 página

Propriedades termodinâmicas de adsorção de água e cinética de secagem de subprodutos da industrialização de abacaxi (Ananás comosus L.): casca e cilindro central

O Brasil tem se mantido nos últimos anos entre os países de maior produção de abacaxi. Em 2009 o país foi o sexto maior produtor deste fruto. Entretanto, devido à alta perecibilidade e às condições de manuseio, altos índices de perdas são verificados durante toda a cadeia de produção, transporte, comercialização e industrialização. Por estas razões, este trabalho teve como objetivo obter as propriedades termodinâmicas de adsorção e a cinética de secagem da casca e cilindro central de abacaxi, fornecendo informações úteis para o aproveitamento desses resíduos. Isotermas de adsorção da casca e do cilindro central de abacaxi foram determinadas pelo método estático gravimétrico nas temperaturas de 40, 50, 60 e 70 °C. Os dados experimentais das isotermas foram ajustados com os modelos de GAB, Henderson, Ferro-Fontan, Peleg, Oswin e Halsey. O modelo de GAB foi o modelo que melhor representou as isotermas de adsorção da casca e cilindro central de abacaxi. Propriedades termodinâmicas de adsorção foram determinadas pela aplicação da equação de Clausius-Clapeyron. Os valores da entalpia de adsorção decresceram com a elevação do teor de umidade. O processo de adsorção da casca de abacaxi apresentou duas zonas de compensação entalpia-entropia, uma entrópica e outra entálpica e o processo de adsorção do cilindro central apenas uma zona entálpica. Os experimentos de secagem da casca e do cilindro foram realizados em um secador convectivo de circulação de ar. Três velocidades de ar (1, 2 e 3 m/s) e quatro temperaturas (40, 50, 60 e 70 °C) foram utilizadas. Aos dados experimentais de secagem foram ajustados o modelo de Fick e os modelos empíricos de Lewis, Page e Henderson-Pabis. O modelo de Fick ajustou-se com qualidade aos dados experimentais...Brazil has maintained in recent years among the countries with the largest pineapple production. In 2009, the country was the sixth largest producer of this fruit. However, due to the high perishability and handling conditions, high percentages of losses are observed throughout the whole production chain. For these reasons the aims of this work were to obtain the adsorption thermodynamic properties and the drying kinetics of the pineapple shell and central cylinder as these information that are useful for the utilization of this waste. The pineapple shell and central cylinder adsorption isotherms were determined by the static gravimetric method under 40, 50, 60 and 70 °C. Six sorption isotherm equations – GAB, Henderson, Ferro-Fontan, Peleg, Oswin and Halsey – were tested to fit adsorption isotherm data. The model that best represented the adsorption isotherms of the pineapple shell and central cylinder was the GAB model. Adsorption thermodynamic properties were determined by applying the Clausius-Clapeyron equation. The adsorption enthalpy values decreased as the moisture content increases. The pineapple shell adsorption process presented two compensation enthalpy-entropy zones, one driven by entropy and other controlled by enthalpy while the adsorption process of pineapple central cylinder presented only one zone driven by the enthalpy. The drying experiments pineapple shell and central cylinder were carried out in a convective dryer of air circulation. Three air velocities (1, 2 and 3 m/s) and four temperatures (40, 50, 60 and 70 °C) were used. Experimental data of drying kinetics were fitted with the Fick model and three empirical models such as Lewis, Page and Henderson-Pabis. The Fick model suited with quality to the experimental data with determination coefficients higher than... (Complete abstract click electronic access below)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP

Extração sequencial de compostos bioativos de subprodutos industriais de maracujá amarelo (Passiflora edulis sp.) utilizando fluidos pressurizados

Orientador: Julian MartínezTese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de AlimentosResumo: Este trabalho teve como objetivo propor processos sequenciais para a obtenção de frações de extrato com propriedades bioativas a partir de resíduos industriais de maracujá amarelo ("Passiflora edulis sp."). A motivação deste tema se fundamenta em dois pilares: i) o aproveitamento e a agregação de valor aos resíduos da industrialização de maracujá; e ii) a extração de compostos bioativos de matrizes vegetais utilizando técnicas limpas e de baixo impacto ambiental. As matérias-primas utilizadas foram bagaço e casca do maracujá amarelo. O bagaço, previamente desidratado e moído, foi submetido à extração com fluido supercrítico (SFE), em que pressão (17, 26 e 35 MPa) e temperatura (40, 50 e 60 ºC) foram as variáveis testadas, e dióxido de carbono (CO2) foi o solvente utilizado. Este estudo de SFE mostrou que diferentes condições de processo permitiram obter extratos com diferente composição química, possibilitando o desenvolvimento sequencial de extrações. A sequência de extrações foi realizada e se obteve três frações de extratos concentradas em: tocóis (60 °C e 17 MPa), ácidos graxos poli-insaturados (50 °C e 17 MPa) e carotenoides (60 °C e 26 MPa). Extração com líquido pressurizado (PLE), a 10 MPa, foi aplicada à matéria-prima submetida previamente à SFE. Misturas de etanol e água (50, 75 e 100%, m/m) e temperatura (50, 60 e 70 °C) foram as variáveis testadas. A condição de extração que resultou em melhores resultados, em termos de rendimento global, obtenção de compostos fenólicos e conteúdo de piceatanol, foi 70 °C e 75% (m/m) de etanol. A etapa prévia de SFE exerceu papel importante na PLE, pois possibilitou obtenção maior rendimento de compostos alvo. Os extratos do bagaço, obtidos por SFE, foram submetidos a ensaios de capacidade antioxidante pelos métodos de captura do radical livre 2,2-diphenyl-1-picrylhydrazyl (DPPH) e Oxygen Radical Absorbance Capacity (ORAC), e os obtidos por PLE, foram analisados por ensaios DPPH, ORAC e Ferric Reducing Ability of Plasma (FRAP). Todos os extratos apresentaram capacidade antioxidante. Altas e positivas correlações foram obtidas entre a capacidade antioxidante e conteúdo total de tocóis, conteúdo de fenólicos totais e conteúdo de piceatanol. A casca, previamente desidratada e moída, foi submetida à SFE, no entanto, não resultou na obtenção de extrato, e por essa razão apenas experimentos de PLE foram realizados. Temperaura (30, 45 e 60 °C) e percentagem de etanol em água como solvente (70, 85 e 100%, v/v) foram as variáveis testadas. Os resultados mostraram a condição de 60 °C e 70% (v/v) como a melhor para obter compostos fenólicos, entre eles, isoorientina, vicenina, orientina, isovitexina e vitexina foram identificados e quantificados. A capacidade antioxidante foi medida pelos métodos DPPH, FRAP e ORAC. O conteúdo dos compostos fenólicos apresentou altos valores de correlação positiva com os ensaios de capacidade antioxidante. Em ambos os processos, do bagaço e da casca, as extração a alta pressão foram comparadas com técnicas de extração a baixa pressão, como Soxhlet e maceração, e nas respostas obtidas, a SFE e a PLE apresentaram melhor desempenho. Avaliação econômica foi realizada para o processo de extração sequencial aplicado ao bagaço e para a PLE aplicada à casca. O programa SuperPro Designer 9.0® foi utilizado nas simulações. A produção das frações de extrato do bagaço e do extrato da casca se mostrou economicamente aplicável, especialmente, quando os extratos são obtidos em larga escala (extrator com capacidade maior que 50 L) e comercializados sob os valores atuais de mercado, preço médio de US$230,00/kg de extrato do bagaço e US$ 125,00/kg de extrato da casca. Menores custos de manufatura foram obtidos na maior escala de produção simulada, i.e., plantas contendo dois extratores de 500 L. A partir dos resultados obtidos neste trabalho, conclui-se que processos sequenciais baseados em extrações com fluidos supercríticos e líquidos pressurizados se mostram viáveis para recuperar compostos de matrizes vegetais, cuja composição apresenta compostos de diferentes polaridades. Desta forma, processos sequenciais de extração se mostram como alternativa para compor o aproveitamento integral das matérias-primas. A obtenção de extratos bioativos dos resíduos do maracujá amarelo pelas técnicas indicadas neste trabalho representa uma oportunidade de aplicação nas indústrias de alimentos, nutracêutica e de cosméticosAbstract: This work aimed to propose sequential processes for obtaining bioactive extract fractions from the industrial waste of yellow passion fruit ("Passiflora edulis sp."). The motivation of this theme is based on: i) to use and to add value to wastes produced during the passion fruit processing; and ii) the extraction of bioactive compounds from plant matrices using clean techniques. Bagasse and rinds were the used raw material. The bagasse, which was previously dried and ground, was submitted to supercritical fluid extraction (SFE). Pressure (17, 26 and 35 MPa) and temperature (40, 50 e 60 ºC) were the variables, and carbon dioxide (CO2) was used as the solvent. This step of SFE showed that different process conditions allowed obtaining extracts with different chemical composition. The sequence of extractions was performed and it was obtained three extract fractions concentrated in tocols (60 °C and 17 MPa), polyunsaturated fatty acids (50 °C and 17 MPa) and carotenoids (60 °C and 26 MPa). Extraction with pressurized liquid (PLE), at 10 MPa, was applied to the raw material that previously was submitted to SFE. Mixtures of ethanol and water (50, 75 and 100%, m/m) and temperature (50, 60 and 70 °C) were the variables. The condition that presented the best results, in terms of global yield, total phenolic content and piceatannol content, was 70 °C and 75% ethanol (m/m). The previous steps of SFE played an important role in the PLE because allowed to obtain a high yield of target compounds. The bagasse extracts, obtained by SFE, were evaluated by 2,2-diphenyl-1-picrylhydrazyl (DPPH) and oxygen radical absorbance capacity (ORAC) assays, and the rind extracts, obtained by PLE, were evaluated by DPPH, ORAC and ferric reducing ability of plasma (FRAP). All the extracts presented antioxidant capacity. High and positive correlations were obtained between antioxidant capacity and total tocol content, total phenolic content, and piceatannol content. The rind, which was previously dried and ground, was submitted to SFE, however, this process did not obtain extract, and for this reason, only the PLE was applied. Temperature (30, 45 and 60 °C) and percentage of ethanol in water (70, 85 and 100%, v/v) were the variables. The results showed 60 °C and 70% (v/v) as the best condition to obtain phenolic compounds, among them, isoorientin, vicenin, orientin, isovitexin and vitexin were identified and quantified. The antioxidant capacity was measured by DPPH, FRAP, and ORAC. The content of phenolic compounds presented high and positive correlation with antioxidant capacity. For both raw materials, bagasse and rind, extractions at high pressure were compared with low-pressure techniques, as Soxhlet and maceration, and SFE and PLE presented a better performance for the evaluated responses. The sequential extraction process applied to the bagasse, and PLE applied to the rinds were submitted to economic analyses using the SuperPro Designer 9.0® software. Producing extracts fractions from bagasse and extract from rind showed economically applicable, especially when the extracts were obtained in large scale (extractor capacity higher than 50 L) and commercialized at an average price of US$230.00/kg bagasse extract and at US$ 125.00/kg rind extract. The lowest costs of manufacturing were obtained for the biggest simulated production scale, i.e., for plants composed by two extractors of 500 L. From the obtained results, it was concluded that sequential processes based on SFE and PLE are viable to obtain composts from vegetal matrixes, which composition presents compounds with different polarity. Therefore, sequential extraction processes show as an alternative to composing the whole use of raw materials. Obtaining bioactive extracts from passion fruit by-products by the techniques indicated in this work represents an opportunity for using it in the industries of foods, pharmaceutical, and cosmeticDoutoradoEngenharia de AlimentosDoutora em Engenharia de Alimentos2014/00372-8FAPESPCAPE

Trends for the application of passion fruit industrial by-products: a review on the chemical composition and extraction techniques of phytochemicals

This work presents a review on the composition and extraction techniques for recovering phytochemicals from passion fruit by-products. The review approaches on the characteristics of each phytochemical and its benefits to human health. It was observed that the by-products of passion fruit contain a range of interesting substances, and for their recovery the application of environmentally friendly extraction techniques, such as supercritical fluid extraction (SFE) and pressurized liquid extraction (PLE), are suggested as single or sequential procedures. The future perspectives of this review encourage the application of these techniques to a complete recovery of passion fruit by-products55164173COORDENAÇÃO DE APERFEIÇOAMENTO DE PESSOAL DE NÍVEL SUPERIOR - CAPESFUNDAÇÃO DE AMPARO À PESQUISA DO ESTADO DE SÃO PAULO - FAPESP2952/20112014/00372-8; 2013/02203-

Supercritical fluid and pressurized liquid extractions of phytonutrients from passion fruit by-products: economic evaluation of sequential multi-stage and single-stage processes

This work presents the economic evaluation of two processes to obtain: i) four extract fractions from passion fruit bagasse by sequential multi-stage process comprising three steps of supercritical fluid extraction (SFE) and one step of pressurized liquid extraction (PLE); ii) one extract from passion fruit rinds by single-stage PLE process. The economic simulation and sensitivity study were performed for plants containing two extraction vessels of 1, 5, 50 and 500 L. The scale-up led to a decrease in the cost of manufacturing (COM). COMs of extracts from sequential multi-stage and single-stage processes decreased from US$220.51/kg to US$ 26.33/kg and US$71.03/kg to US$ 11.96/kg, respectively, when the system capacity increased from 2 × 1 L to 2 × 500 L. Itemized costs related to materials, facilities, labor and utilities are also presented. Both processes are economically promising, especially when the extracts are produced in large scale and sold by the current market price1228898COORDENAÇÃO DE APERFEIÇOAMENTO DE PESSOAL DE NÍVEL SUPERIOR - CAPESFUNDAÇÃO DE AMPARO À PESQUISA DO ESTADO DE SÃO PAULO - FAPESP2952/20112014/00372-8; 2013/02203-6; 2015/11932-

Sub- and supercritical fluid technology applied to food waste processing

Food industries produce annually billions of tons of non-edible residues, which can cause pollution, management and economic problems worldwide. Environment damages such as water, soil and air contamination are global concerns, and are the main reason for the development of different strategies to use agricultural and industrial residues as source of new products. To apply the food wastes, environment-friendly processes are recommendable, in which renewable sources are used and the products do not offer environmental risks. Sub- and supercritical fluid technologies can meet such requirements when using green solvents. This review gives an overview of the potential of food residues as raw materials for the production of nutritionally interesting compounds, chemicals and biofuels. Aiming to recover components from food residues, processes in which sub- and supercritical technologies can be used, in single or combined ways, are discussed. Several applications are reported96272286CONSELHO NACIONAL DE DESENVOLVIMENTO CIENTÍFICO E TECNOLÓGICO - CNPQCOORDENAÇÃO DE APERFEIÇOAMENTO DE PESSOAL DE NÍVEL SUPERIOR - CAPESFUNDAÇÃO DE AMPARO À PESQUISA DO ESTADO DE SÃO PAULO - FAPESPSem informaçãoSem informação2013/02203-6; 2014/00372-8Workshop on Supercritical Fluids and Energ

Supercritical Carbon Dioxide Technology for Recovering Valuable Phytochemicals from <i>Cannabis sativa</i> L. and Valorization of Its Biomass for Food Applications

Supercritical carbon dioxide (CO2) extraction techniques meet all-new consumer market demands for health-promoting phytochemical compound-rich extracts produced from green and sustainable technology. In this regard, this review is dedicated to discussing is the promise of integrating high-pressure CO2 technologies into the Cannabis sativa L. processing chain to valorize its valuable pharmaceutical properties and food biomass. To do this, the cannabis plant, cannabinoids, and endocannabinoid system were reviewed to understand their therapeutic and side effects. The supercritical fluid extraction (SFE) technique was presented as a smart alternative to producing cannabis bioproducts. The impact of SFE operating conditions on cannabis compound extraction was examined for aerial parts (inflorescences, stems, and leaves), seeds, and byproducts. Furthermore, the opportunities of using non-thermal supercritical CO2 processing on cannabis biomass were addressed for industrial hemp valorization, focusing on its biorefinery to simultaneously produce cannabidiol and new ingredients for food applications as plant-based products