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- Enhancing anthocyanin extraction from wine lees: a comprehensive ultrasound-assisted optimization studyPublication . Umsza-Guez, Marcelo A.; Vázquez-Espinosa, Mercedes; Chinchilla, Nuria; Aliaño-González, M. J.; Oliveira de Souza, Carolina; Ayena, Kodjovi; Fernández Barbero, Gerardo; Palma, Miguel; Carrera, CeferinoWine lees, an important by-product of the wine industry, pose a major environmental problem due to the enormous quantities of solid-liquid waste that are discarded annually without defined applications. In this study, the optimization of a method based on a Box-Behnken design with surface response has been carried out to obtain extracts with high anthocyanin content and potent antioxidant activity. Six variables have been considered: %EtOH, temperature, amplitude, cycle, pH, and ratio. The developed method exhibited important repeatability properties and intermediate precision, with less than 5% CV being achieved. Furthermore, these novel methods were successfully applied to diverse wine lees samples sourced from Cabernet Sauvignon and Syrah varieties (Vitis vinifera), resulting in extracts enriched with significant anthocyanin content and noteworthy antioxidant activity. Additionally, this study evaluated the influence of grape variety, fermentation type (alcoholic or malolactic), and sample treatment on anthocyanin content and antioxidant activity, providing valuable insights for further research and application in various sectors. The potential applications of these high-quality extracts extend beyond the winemaking industry, holding promise for fields like medicine, pharmaceuticals, and nutraceuticals, thus promoting a circular economy and mitigating environmental contamination.
- On the valorization of Arbutus unedo L. Pomace: Polyphenol extraction and development of novel functional cookiesPublication . Duarte, Hugo; Carrera, Ceferino; Aliaño-González, M.J.; Gutiérrez-Escobar, Rocío; Jiménez-Hierro, María Jesús; Palma, Miguel; Galego, Ludovina; Romano, Anabela; Medronho, BrunoThe fruits of Arbutus unedo L. have a crimson colour and are enriched with remarkable concentrations of bioactive compounds such as anthocyanins and polyphenols. These fruits are commonly used in the production of a Portuguese Protected Geographical Indication distillate called “Aguardente de Medronho”. During this process, a solid pomace is generated and presently discarded without valuable applications. In this work, two strategies have been developed for the valorisation of A. unedo pomace. The first approach considers the extraction of polyphenols from this by-product through the optimization of an ultrasound-assisted method using a Box-Behnken design coupled with response surface methodology. The results indicate that the temperature and the percentage of methanol, along with their interaction, significantly influence the total concentration of polyphenols and the antioxidant activity of the extracts obtained. The optimal conditions identified consider the extraction of 0.5 g of sample with 20 mL of a solvent containing 74% MeOH (aq), at a pH of 4.8, maintained at 70 ◦C for 15 min. On the other hand, the second valorisation strategy considered the use of A. unedo pomace in the development of functional cookies. The incorporation of 15–20% pomace in the cookie formulation was well-received by consumers. This incorporation results in an intake of ca. 6.55 mg of polyphenols per gram of cookie consumed, accompanied by an antioxidant activity of 4.54 mg Trolox equivalents per gram of cookie consumed. Overall, these results encourage the employment of A. unedo pomace either as a reliable source of extracts enriched in polyphenols or as a nutraceutical active ingredient in functional cookies, thereby positively impacting human health.
- Ultrasound-assisted extraction of betalains from opuntia fruit pulp of different color varietiesPublication . Vázquez-Espinosa, Mercedes; González-de-Peredo, Ana V.; Carrera, Ceferino; Palma, Miguel; Barbero, Gerardo F.; Aliaño-González, M.J.Betalains are water-soluble pigments that have exhibited important pharmacological properties such as antioxidant, anticancer, antilipidemic and antimicrobial activity. These compounds have been isolated in numerous purple plants or fruits, as is the case of the wild species under the Opuntia genus. The fruits of these species are often disregarded because of their small size as well as the frequent presence of prickles. Based on this, this research has as its objective the optimization of a method based on ultrasound-assisted extraction to obtain extracts enriched with betalains from a wild Opuntia species (Opuntia dillenii (Ker Gawl.) Haw.). Four variables (%EtOH in the solvent, temperature of extraction, ultrasound amplitude and cycle) were selected using a Box-Behnken design. The quadratic interaction of %EtOH and the interaction of %EtOH-cycle have proven to be influential variables at 95% confidence. The conditions to obtain the highest betalain concentration were 100 mg of pulp with 20 mL (60%:40% EtOH:H2O) solvent at 20 degrees C at 24% amplitude and 0.2 cycle for 10 min. The suitability and reliability of the method were evaluated with repeatability and intermediate precision tests obtaining CVs <5%. Finally, the developed method has been employed in the analysis of five Opuntia commercial samples and obtained significant antioxidant activity of the extracts, confirming its applicability.
- Optimization of an Enzyme-Assisted Extraction Method for the Anthocyanins Present in Açai (Euterpe oleracea Mart.)Publication . Alavarsa-Cascales, Diego; Aliaño-González, M.J.; Palma, Miguel; Barbero, Gerardo F.; Carrera, CeferinoSeveral investigations have proven the presence of anthocyanins in different parts of acai plants. These compounds are responsible for the notable therapeutic properties of acai such as antioxidant, antimicrobial, anti-inflammatory, anticancer, and anticonvulsant. We have therefore optimized an enzyme-assisted extraction method for the anthocyanins found in acai, to be subsequently applied in many fields such as agrifood, medicine, or cosmetics. A Plackett-Burman design with seven variables (time of extraction, pH, temperature, agitation, percentage of ethanol in the solvent, amount of sample, and units of enzyme) was employed to determine the predominant extraction variables, of which four were categorized as influential. Subsequently, a Box-Behnken design-response surface methodology made it possible to determine the degree of influence from these variables and their optimal values. The optimal conditions were established as 0.1 g of acai heated up to 60 degrees C and extracted using 15 mL of solvent with pH 4 and 40% ethanol, 500 units of enzyme per gram of sample, and agitation at 150 rpm for 15 min. The repeatability and intermediate precision of the developed method were confirmed by variation coefficients below 5%. Finally, the developed method was compared against the extensively used maceration and ultrasound-assisted extraction methods.
- Enhancing efficiency of enzymatic-assisted extraction method for evaluating bioactive compound analysis in mulberry: an optimization approachPublication . Tizón Alba, Ainara; Aliaño-González, M.J.; Palma, Miguel; Fernández Barbero, Gerardo; Carrera, CeferinoThe present investigation endeavors to optimize a method based on enzyme-assisted extraction for the efficient retrieval of bioactive compounds from mulberry, leveraging its notable health-promoting properties. A combined approach of Plackett-Burman design followed by Box-Behnken design was employed for determining the crucial extraction parameters and subsequently, refining the process. Optimal conditions consisted of heating 0.15 g of mulberry at 40 degrees C, using 15 mL of 70% EtOH as a solvent at pH 4, 38.46 enzyme units per g of sample, and shaking at 200 rpm. The optimum extraction time study revealed that 5 min of extraction was sufficient to reach the maximum concentration of the bioactive compound. The repeatability and intermediate precision assessment exhibited a coefficient of variation below 5%. Among the diverse mulberry varieties scrutinized, Morus nigra showed the highest anthocyanin content (27.90 +/- 2.14 mg/100 g), while Morus rubra showed the highest concentration of phenolic compounds (121.10 +/- 19.56 mg/100 g). Moreover, the extracted compounds showcased significant antioxidant and antimicrobial properties.
- Advancements in detection and mitigation strategies for Petroleum-Derived contaminants in aquatic environments: a comprehensive reviewPublication . Duarte, Hugo; Aliaño González, María José; Medronho, BrunoThe exponential increase in the production and transportation of petroleum-derived products observed in recent years has been driven by the escalating demand for energy, textiles, plastic-based materials, and other goods derived from petroleum. Consequently, there has been a corresponding rise in spills of these petroleum derivatives, particularly in water sources utilized for transportation or, occasionally, illegally utilized for tank cleaning or industrial equipment maintenance. Numerous researchers have proposed highly effective techniques for detecting these products, aiming to facilitate their cleanup or containment and thereby minimize environmental pollution. However, many of these techniques rely on the identification of individual compounds, which presents significant drawbacks, including complexity of handling, subjectivity, lengthy analysis times, infeasibility for in situ analysis, and high costs. In response, there has been a notable surge in the utilization of sensors or generalized profiling techniques serving as sensors to generate characteristic fingerprints of these products, thereby circumventing the aforementioned disadvantages. This review comprehensively examines the evolution of techniques employed for detecting petroleum-derived products in water samples, along with their associated advantages and disadvantages. Furthermore, the review examines current perspectives on methods for the removal and/or containment of these products from water sources, to minimize their environmental impact and the associated health repercussions on living organisms and ecosystems.
- Enhancing cellulose and lignin fractionation from acacia wood: optimized parameters using a deep eutectic solvent system and solvent recoveryPublication . Magalhães, Solange; Aliaño González, María José; Rodrigues, Mariana; Fernandes, Catarina; Mendes, Cátia V. T.; Carvalho, Maria Graça V. S.; Alves, Luís; Medronho, Bruno; Rasteiro, Maria da GraçaCellulose and lignin, sourced from biomass, hold potential for innovative bioprocesses and biomaterials. However, traditional fractionation and purification methods often rely on harmful chemicals and high temperatures, making these processes both hazardous and costly. This study introduces a sustainable approach for fractionating acacia wood, focusing on both cellulose and lignin extraction using a deep eutectic solvent (DES) composed of choline chloride (ChCl) and levulinic acid (LA). A design of experiment was employed for the optimization of the most relevant fractionation parameters: time and temperature. In the case of the lignin, both parameters were found to be significant variables in the fractionation process (p-values of 0.0128 and 0.0319 for time and temperature, respectively), with a positive influence. Likewise, in the cellulose case, time and temperature also demonstrated a positive effect, with p-values of 0.0103 and 0.028, respectively. An optimization study was finally conducted to determine the maximum fractionation yield of lignin and cellulose. The optimized conditions were found to be 15% (w/v) of the wood sample in 1:3 ChCl:LA under a treatment temperature of 160 degrees C for 8 h. The developed method was validated through repeatability and intermediate precision studies, which yielded a coefficient of variation lower than 5%. The recovery and reuse of DES were successfully evaluated, revealing remarkable fractionation yields even after five cycles. This work demonstrates the feasibility of selectively extracting lignin and cellulose from woody biomass using a sustainable solvent, thus paving the way for valorization of invasive species biomass.
- Lignin extraction from acacia wood: crafting deep eutectic solvents with a systematic D-optimal mixture-process experimental designPublication . Fernandes, Catarina; Aliaño González, María José; Gomes, Leandro Cid; Bernin, Diana; Gaspar, Rita; Fardim, Pedro; Reis, Marco S.; Alves, Luís; Medronho, Bruno; Rasteiro, Maria Graça; Varela, CarlaLignin is a complex biopolymer whose efficient extraction from biomass is crucial for various applications. Deep eutectic solvents (DES), particularly natural-origin DES (NADES), have emerged as promising systems for lignin fractionation and separation from other biomass components. While ternary DES offer enhanced fractionation performance, the role of each component in these mixtures remains unclear. In this study, the effects of adding tartaric acid (Tart) or citric acid (Cit) to a common binary DES mixture composed of lactic acid (Lact) and choline chloride (ChCl) were investigated for lignin extraction from acacia wood. Ternary Cit-based DES showed superior performance compared to Tart-based DES. Using a combined mixture-process D-Optimal experimental design, the Lact:Cit:ChCl DES composition and extraction temperature were optimized targeting maximum lignin yield and purity. The optimal conditions (i.e., Lact:Cit:ChCl, 0.6:0.3:0.1 molar ratio, 140 degrees C) resulted in a lignin extraction yield of 99.63 +/- 1.24 % and a lignin purity of 91.45 +/- 1.03 %. Furthermore, this DES exhibited feasible recyclability and reusability without sacrificing efficiency.
- Development of a new eco-friendly ultrasound-assisted extraction method to quantify tryptophan in wild mushrooms and determination of its beneficial propertiesPublication . López, Alejandro R.; Ortega-Caneda, Elena; Espada-Bellido, Estrella; Chinchilla, Nuria; Palma, Miguel; Aliaño González, María José; Barbero, Gerardo Fernández; Carrera, CeferinoBioactive compounds in food offer health benefits by influencing cellular and physiological functions. Tryptophan, an essential amino acid and precursor to neurotransmitters like melatonin and serotonin, regulates mood and circadian rhythms. However, its quantification in mushrooms is scarce studied. An eco-friendly ultrasound- assisted extraction (UAE) method has been optimized to quantify tryptophan using ultra high-performance liquid chromatography with a diode array and fluorescence detector (UHPLC-DAD-Fl). Tryptophan levels were determined in 26 wild mushroom samples of the genus Lactarius and Boletus. The concentrations ranged from 0.042 mg/g to 0.742 mg/g. The extracts' health benefits were assessed for antioxidant capacity using DPPH (17.7 %71.6 %) and ABTS (7.2 %24.9 %) methods, while acetylcholinesterase (AChE) inhibitory activity ranged from 13.1 % to 49.8 %. Promising results were obtained. Hierarchical cluster analysis demonstrated a correlation between tryptophan concentration, mushroom species, location, and extract properties, highlighting tryptophan's crucial role in these mushrooms' health benefits.
- Lignin-furanic rigid foams: Enhanced methylene blue removal capacity, recyclability, and flame retardancyPublication . Duarte, Hugo; Brás, João; Saoudi Hassani, El Mokhtar; Aliaño González, María José; Magalhães, Solange; Alves, Luís; Valente, Artur J. M.; Eivazi, Alireza; Norgren, Magnus; Romano, Anabela; Medronho, BrunoWorldwide, populations face issues related to water and energy consumption. Water scarcity has intensified globally, particularly in arid and semiarid regions. Projections indicate that by 2030, global water demand will rise by 50%, leading to critical shortages, further intensified by the impacts of climate change. Moreover, wastewater treatment needs further development, given the presence of persistent organic pollutants, such as dyes and pharmaceuticals. In addition, the continuous increase in energy demand and rising prices directly impact households and businesses, highlighting the importance of energy savings through effective building insulation. In this regard, tannin-furanic foams are recognized as promising sustainable foams due to their fire resistance, low thermal conductivity, and high water and chemical stability. In this study, tannin and lignin rigid foams were explored not only for their traditional applications but also as versatile materials suitable for wastewater treatment. Furthermore, a systematic approach demonstrates the complete replacement of the tannin-furan foam phenol source with two lignins that mainly differ in molecular weight and pH, as well as how these parameters affect the rigid foam structure and methylene blue (MB) removal capacity. Alkali-lignin-based foams exhibited notable MB adsorption capacity (220 mg g−1), with kinetic and equilibrium data analysis suggesting a multilayer adsorption process. The prepared foams demonstrated the ability to be recycled for at least five adsorption-desorption cycles and exhibited effective flame retardant properties. When exposed to a butane flame for 5 min, the foams did not release smoke or ignite, nor did they contribute to flame propagation, with the red glow dissipating only 20 s after flame exposure.