Search Results (61)

This study aimed to optimize the ultrasound-assisted extraction (UAE) process using food-grade ethanol to recover glucosinolates from upcycled cauliflower through response surface methodology. The optimized extraction process was compared with traditional extraction using maceration with solvents such as methanol and acetone. The optimum UAE conditions identified for extracting glucosinolates from upcycled cauliflower were: 42% ethanol as solvent at 43 °C for 30 min. The total glucosinolate content recovered was 7400 μg sinigrin equivalence (SE)/g dry weight (DW) of biomass. The ultra-pressure liquid chromatography–electrospray ionization-mass spectrometry (UPLC-ESI-MS) analysis confirmed that the optimized UAE yielded the highest levels of glucoraphanin (1.31 ± 0.12 μg/g DW of biomass) and sulforaphane (28.2 ± 3.34 μg/g DW of biomass). The extracts possess greater antioxidant activity as determined by ferric reducing antioxidant power and DPPH radical scavenging activity. The optimized UAE process significantly enhanced the extraction of valuable phytochemical molecules from the upcycled cauliflower. Further studies should focus on evaluating their therapeutic and preventive potential for applications in nutrition and health. Full article

Macroalgae (seaweeds) represent a sustainable and alternative source of high-value fatty acids (FAs), including omega-3 (n-3) and omega-6 (n-6), which could help alleviate pressure on wild fish stocks and mitigate global overfishing. This study analyzed the FA composition of field-collected red (Chondracanthus acicularis, Ballia callitriche, Gracilaria sp., and Gelidium coulteri), brown (Padina pavonica, Sargassum vulgare, Cystoseira myrica, Cystoseira sp., Dictyota dichotoma, and Stephanocystis mundane), and green seaweeds (Ulva compressa). Additionally, lipid extraction was optimized using food-grade solvents, reaction temperatures, and the functional properties of selected green and brown seaweeds. The results showed that brown and green seaweeds contained higher total FA content than red seaweeds, with a favorable n-6/n-3 ratio below 10. The selected species’ functional properties (Water- and Oil-Holding Capacities, Swelling Capacity) met food-grade standards. Ethyl acetate at 60 °C was identified as the optimal food-grade solvent for lipid extraction. Functional properties varied significantly by species and processing conditions, with Ulva compressa exhibiting superior Water- and Oil-Holding Capacities and Swelling Capacity compared to Cystoseira myrica, highlighting its potential as a functional food ingredient. These findings support using seaweeds as a sustainable source for human nutrition. Full article

Food waste has a significant social impact but can be revalued as a source of bioactive compounds, such as condensed tannins. This abundant biomass, corresponding to a polymeric antioxidant, must be depolymerized to become bioavailable. Previous studies have investigated polymer degradation into oligomers using high temperatures and expensive nucleophiles, often under conditions unsuitable for food applications. In the present investigation, it is proposed that the depolymerization of condensed tannins can occur under food-grade conditions using a Generally Recognized as Safe (GRAS) solvent by optimizing the reaction’s heating method with microwave assistance and using gallic acid as a nucleophile. Thermal studies indicate that the degradation of total polyphenols content follows first-order kinetics and occurs above 80 °C in microwave. Depolymerization follows second-order kinetics, yielding epicatechin as the primary product with zero-order formation kinetics. The optimized factors were 80% v/v ethanol, 10 mg/mL polymeric tannins, and 5.88 mg/mL gallic acid. Under these conditions, the reaction efficiency was 99.9%, the mean particle diameter was 5.7 nm, the total polyphenols content was 297.3 ± 15.9 EAG mg/g, and the inhibition of ABTS●+ and DPPH● radicals was 93.5 ± 0.9% and 88.2 ± 1.5%, respectively. These results are promising for future scaling processes. Full article

Haskap (Lonicera caerulea) berry is rich in anthocyanins, particularly cyanidin-3-O-glucoside (C3G). In this investigation, a response surface methodology was applied to optimize the anhydrous ethanol-based extraction parameters to obtain the maximum yield of anthocyanins from haskap berry and to compare the recovery of anthocyanins from different extraction methods. The central composite design was employed to study the effect of three independent variables (X_A = ultrasonic bath power, X_B = extraction temperature, and X_C = extraction time) which were found to significantly affect the response variable total anthocyanin content (TAC) and fit to the second-order polynomial model. The optimum process parameters of X_A = 536 W, X_B = 62.3 °C, and X_C = 63.5 min provided a predicted TAC of 16.5 mg C3G equivalence (C3GE)/g dry weight (DW), which was experimentally validated with 16.1 mg of C3GE/g DW. The optimized ultrasonication-assisted extraction process using anhydrous ethanol was also effective in recovering quercetin glycosides, catechin, procyanidin B2, and iridoids, as determined by ultra-pressure liquid chromatography–mass spectrometry. Though the anthocyanin recovery was the highest (17.6 mg of C3GE/g DW) when a deep eutectic solvent consisting of citric acid and D-(+)-maltose was used, this solvent system has limitations when preparing dehydrated extracts for industrial applications. This study concludes that the effective extraction of anthocyanins and other phytochemicals from haskap berries can be performed using food-grade anhydrous ethanol. Full article

The tomato (Lycopersicon esculentum) is a prominent fruit in Mediterranean countries with established biological activities for consumers. Given the widespread distribution of the fruit and its large production, the need to utilize the by-products seems imperative. With a view to valorizing the main carotenoid of tomato processing industry waste, lycopene, as well as other bioactive compounds (i.e., polyphenols), the optimization of a green extraction method involving ultrasound-assisted bath extraction (UBAE) was carried out. The results showed that the optimized UBAE technique achieved substantial yields of total carotenoids (420.8 μg of lycopene equivalents per gram of dry weight (dw)) and total polyphenols (2.62 mg of gallic acid equivalents per gram of dw). Flavonoid naringin (0.48 mg/g dw) and non-flavonoid coniferyl alcohol (0.32 mg/g dw) were the most abundant identified polyphenols. However, comparison with a conventional stirring extraction revealed that the latter technique marked double figures in all assays, including antioxidant activity assays. The study revealed that UBAE was not a preferable technique for recovering carotenoids because of the possible degradation of labile compounds found in tomato processing industry waste. Given that the extraction solvent was pure ethanol, the study established a foundation for the development of a unique lycopene-enriched product in the food industry. It is essential to conduct additional studies using alternative food-grade solvents or other environmentally friendly extraction methods. Full article

This study aims to evaluate the effectiveness of microwave-assisted and conventional extraction using ethanol, hexane, and petroleum ether as solvents, and to optimize the process for extracting oil from Moringa oleifera Lam. seeds, with a focus on improving food-grade oil production. Response surface methodology (RSM) was applied to enhance the extraction process of the oil. Central composite rotational design (CCRD) was used to analyze the impact of solid–liquid ratio (x₁), power (x₂), and temperature (x₃) on oil yield. The optimization identified the optimal conditions as a solid/liquid ratio of 1:38, power of 175 W, and temperature of 50 °C, achieving a 42% oil yield. Notably, the microwave-assisted extraction reduced the processing time from 8 h (using conventional Soxhlet extraction) to just 1 h. Conventional extraction with hexane and petroleum ether was also performed for comparison, resulting in similar oil content and fatty acid profiles, predominantly, oleic acid. FTIR analysis confirmed that the microwave-extracted oil contained fatty acids and had similar characteristics to the conventionally extracted oil. Thus, the use of ethanol as a green solvent in the microwave has shown significant improvement in terms of time and energy savings compared to the Soxhlet method with toxic solvents. This study concludes that microwave-assisted extraction with ethanol provides a more energy efficient, environmentally friendly, and time-saving alternative for food-grade oil production, aligning with advancements in food engineering and production. Full article

Inspired by the proved dissolving power of vegetable oils for non-polar and low-polar natural compounds, animal fats with triglycerides as the major components were investigated as food-grade solvents in this study for the simultaneous extraction of carotenoids and capsaicinoids from Sichuan chili. The dissolving power of lard, beef tallow, chicken fat and basa fish oil in the extraction of er jing tiao chili was firstly compared, where animal oils with worse extraction ratios for carotenoids (0.79 mg/g in average) performed better for the extraction of capsaicinoids (0.65 mg/g in average). Furthermore, the solvent effect of animal fats on the oleo-extracts was evaluated in terms of fatty acid composition, oil quality indexes, crystal polymorphism, melting and crystallization behaviors, where no significant differences were observed between animal fats before and after extraction. The oxidative stability of animal fats could be 1.02- up to 2.73-fold enhanced after extraction and the pungency degree could reach the same spicy level as commercial hotpot oil. In addition, the Hansen solubility parameters of solvents and solutes were predicted for further theoretical miscibility study, which helps to make a better comprehension of the dissolving mechanism behind such oleo-extraction. Overall, animal fats demonstrated their considerable solvent power for extracting carotenoids and capsaicinoids simultaneously from Sichuan chili, which showed significant potential for developing a novel Sichuan spicy hotpot oil with enhanced flavor and stability. Full article

Monitoring plasma concentrations of β-lactam antibiotics is crucial, particularly in critically ill patients, where variations in concentrations can lead to treatment failure or adverse events. Standardized antimicrobial regimens may not be effective for all patients, especially in special groups with altered physiological parameters. Pharmacokinetic/pharmacodynamic (PK/PD) studies highlight the time-dependent antibacterial activity of these antibiotics, emphasizing the need for personalized dosing. Therapeutic drug monitoring (TDM) is essential, requiring rapid and accurate analytical methods for precise determination of drugs in biological material (typically plasma or serum). This study presents a novel capillary zone electrophoresis–tandem mass spectrometry (CZE-MS/MS) method designed for the simultaneous quantification of five penicillin antibiotics, two cephalosporins, one carbapenem, and two β-lactamase inhibitors in a single run. The method involves a simple sample pretreatment—precipitation with organic solvent—and has a run time of 20 min. Optimization of CZE separation conditions revealed that 20 mM ammonium hydrogen carbonate (NH₄HCO₃) serves as the optimal background electrolyte (BGE). Positive electrospray ionization (ESI) mode, with isopropyl alcohol (IP)/10 mM ammonium formate water solution (50/50, v/v) as the sheath liquid, was identified as the optimal condition for MS detection. Method validation according to the Food and Drug Administration (FDA) guideline for development of bioanalytical methods demonstrated satisfactory selectivity, linearity, recovery, robustness, and stability. The method’s practicality was evaluated using the Blue Applicability Grade Index (BAGI), yielding a score of 77.5. Moreover, the greenness of the proposed method was evaluated by two commonly used metric tools—Analytical GREEnness (AGREE) and Green Analytical Procedure Index (GAPI). The developed CZE-MS/MS method offers a practical and reliable approach for quantifying a broad spectrum of β-lactam antibiotics in plasma. Its ability to simultaneously quantify multiple analytes in a single run, coupled with a straightforward sample pretreatment, positions it as a valuable and prospective tool for TDM in critically ill patients. Full article

Lutein, a yellow xanthophyll carotenoid, is increasingly recognized for its nutraceutical benefits, particularly in protecting the retina’s macula from age-related degeneration. Microalgae are a promising source of lutein, which can be a primary product or a coproduct in biorefineries. Certain microalgae exhibit lutein levels (up to 1.7%) surpassing those of common dietary sources like kale, spinach, and egg yolk (approximately 0.7–0.9%). Predominantly associated with photosystem II’s light-harvesting complex, lutein is crucial in photosynthesis and cellular defense. However, being quantitatively minor among cellular constituents, lutein necessitates specialized processing for efficient extraction. Although ubiquitous in microalgae, it is not as easily inducible as β-carotene and astaxanthin in Dunaliella salina and Haematococcus pluvialis, respectively. Currently, microalgal lutein production predominantly occurs at the bench scale, presenting challenges in scaling up. Factors like culture medium significantly influence biomass and lutein yields in industrial production, while downstream processing requires cost-effective, food-grade solvent extraction techniques. This review delves into contemporary methods and innovative progress in microalgal lutein production, emphasizing industrial-scale processes from biomass cultivation to final product formulation. A conceptual industrial process proposed in this review shows that two 10 m³ photobioreactors could produce 108 kg dry mass for Chlorella minutissima, which can be processed into approximately 616 g of lutein extract, or over 6000 capsules of finished nutraceutical daily. Despite lutein production via microalgae being in nascent stages at large scales, existing research provides a solid foundation for well-informed scale-up endeavors. Full article

Brown macroalgae are rich sources of nutrients and health-promoting compounds. Nevertheless, their consumption is still limited by their strong organoleptic characteristics, thus requiring the development of extraction strategies to profit from their nutritional value. To fulfil this, two sequential extraction approaches were developed, differing in the solvent used in the first extraction step, water in approach 1 or food-grade ethanol in approach 2, to obtain economic and affordable extracts rich in specific compounds from Fucus vesiculosus. The use of water in the first step of extraction allowed us to recover water-soluble phlorotannins, laminarans and mannuronic-rich alginates, making the subsequent 70% ethanol extract richest in fucoxanthin (0.07% algae DW), and the hot water fractions purest in fucoidans and alginates with a lower mannuronic-to-guluronic (M/G) ratio (2.91). Conversely, when beginning extraction procedures with 96% ethanol, the recovered yields of phlorotannins increased (0.43 g PGE/100 g algae DW), but there was a concomitant seven-fold decrease in the recovery of fucoxanthin in the subsequent 70% ethanol extract. This approach also led to less pure hot water fractions containing fucoidans, laminarans and alginates with a higher M/G ratio (5.50). Overall, this work unveiled the potential of the first extraction steps in sustainable and holistic cascade strategies to modulate the composition of food-grade extracts, creating prospects of their application as tailored functional ingredients in food products. Full article

Olive pomace results from the production of olive oil. Even if olive pomace represents a potential environmental problem, it contains phenolic compounds, which are widely recognized for their beneficial properties for human health. In this study, an innovative and sustainable technological approach to extract phenolic compounds from fresh olive pomace, based on food-grade solvent instead of those usually adopted, is investigated. Characterization and shelf-life evaluation of the hydroalcoholic extracts obtained from the procedure developed for different industrial purposes were also carried out. The phenolic fractions of the different samples were studied with the Folin–Ciocâlteu method to quantify that the total reducing molecules and HPLC-MS/MS analysis was used to define the profile through the identification and quantification of 42 compounds, belonging to five chemical families. Regarding shelf-life, the hydroalcoholic extract showed no significant reduction in phenolic content, for both instrumental evaluations, retaining most of the phenolic compounds present in the raw material; negative attributes were not perceived by sensory evaluation. Thus, these lab-scale results can be the starting point to develop a procedure that is suitable for a real olive mill, representing a valorization strategy in a circular economy and the perspective of new business models. Full article

Polyphenols from residual non-food grade Salicornia ramosissima have health-promoting effects in feed, food, or nutraceutical applications. Therefore, the isolation of polyphenols is of interest from a series of environmentally friendly isolation methods with recyclable solvents. The isolation of polyphenols from non-food grade S. ramosissima was investigated using sequential membrane filtration with and without acid pretreatment, liquid–liquid extraction, resin adsorption, and centrifugal partition chromatography (CPC); analyzed by the Folin–Ciocalteu assay for total polyphenols; and finally analyzed using UPLC-TQMS in negative ion-spray mode for detection of 14 polyphenols. Sequential membrane filtration and acid hydrolysis indicated the polyphenols forming complexes with other compounds, retaining the polyphenols in the retentate fraction of large molecular weight cut-off membrane sizes. Conventional liquid–liquid extraction using sequential ethyl acetate and n-butanol showed most polyphenols were extracted, apart from chlorogenic acids, indicating a low isolation efficiency of higher polarity polyphenols. Analysis of the extract after resin adsorption by Amberlite XAD-4 resin showed high efficiency for separation, with 100% of polyphenols adsorbed to the resin after 13 bed volumes and 96.7% eluted from the resin using ethanol. CPC fractionations were performed to fractionate the concentrated extract after resin adsorption. CPC fractionations of the 14 polyphenols were performed using an organic or aqueous phase as a mobile phase. Depending on the mobile phase, different compounds were isolated in a high concentration. Using these easily scalable methods, it was possible to comprehensively study the polyphenols of interest from S. ramosissima and their isolation mechanics. This study will potentially lead the way for the large-scale isolation of polyphenols from S. ramosissima and other complex halophytes. The compounds of the highest concentration after CPC fractionation were isoquercitrin and hyperoside (155.27 mg/g), chlorogenic acid (85.54 mg/g), cryptochlorogenic acid (101.50 mg/g), and protocatechuic acid (398.67 mg/g), and further isolation using CPC could potentially yield novel polyphenol nutraceuticals. Full article

Conventionally, methanol is the solvent of choice in the synthesis of gamma-cyclodextrin metal-organic frameworks (γ-CD-MOFs), but using ethanol as a replacement could allow for a more food-grade synthesis condition. Therefore, the aim of the study was to compare the γ-CD-MOFs synthesised with both methanol and ethanol. The γ-CD-MOFs were characterised by scanning electron microscopy (SEM), surface area and pore measurement, Fourier transform infrared spectroscopy (FTIR) and powder X-ray diffraction (PXRD). The encapsulation efficiency (EE) and loading capacity (LC) of the γ-CD-MOFs were also determined for curcumin, using methanol, ethanol and a mixture of the two as encapsulation solvent. It was found that γ-CD-MOFs synthesised by methanol and ethanol do not differ greatly, the most significant difference being the larger crystal size of γ-CD-MOFs crystallised from ethanol. However, the change in solvent significantly influenced the EE and LC of the crystals. The higher solubility of curcumin in ethanol reduced interactions with the γ-CD-MOFs and resulted in lowered EE and LC. This suggests that different solvents should be used to deliberately manipulate the EE and LC of target compounds for better use of γ-CD-MOFs as their encapsulating and delivery agents. Full article

This study assessed the halophyte species Limonium spathulatum (Desf.) as a possible source of natural ingredients with the capacity to inhibit enzymes related to relevant human health disorders and food browning. Extracts using food-grade solvents such as water and ethanol were prepared by maceration from dried L. spathulatum leaves. They were evaluated for in vitro inhibition activity of enzymes such as acetylcholinesterase (AChE) and butyrylcholinesterase (BChE), α-glucosidase, tyrosinase and lipase, related to Alzheimer’s disease, type-2-diabetes mellitus, skin hyperpigmentation, and obesity, respectively. These extracts were also appraised for in vitro acute toxicity on tumoral and non-tumoral cell lines and their chemical composition by high-performance liquid chromatography coupled with electrospray ionization mass spectrometry (HPLC-ESI-MS/MS). The extracts were more effective towards BChE than AChE. The best results were obtained with the hydroethanolic and water extracts, with IC₅₀ values of 0.03 mg/mL and 0.06 mg/mL, respectively. The hydroethanolic extract had the highest capacity to inhibit α-glucosidase (IC₅₀: 0.04 mg/mL), higher than the positive control used (acarbose, IC₅₀ = 3.14 mg/mL). The ethanol extract displayed the best inhibitory activity against tyrosinase (IC₅₀ = 0.34 mg/mL). The tested samples did not inhibit lipase and exhibited low to moderate cytotoxic activity against the tested cell lines. The hydroethanolic extract had a higher diversity of compounds, followed by the ethanol and water samples. Similar molecules were identified in all the extracts and were mainly hydroxybenzoic acids, hydroxycinnamic acids, and flavonoids. Taken together, these results suggest that L. spathulatum should be further explored as a source of bioactive ingredients for the food, cosmetic, and pharmaceutical industries. Full article

Bioactive peptides derived from fish the byproduct protein hydrolysate have wide potential as functional food ingredients. The preparation of bioactive peptides is commonly achieved via enzymatic hydrolysis; this is the most preferred method because it has high specificity, fewer residual organic solvents in the product, and it is usually carried out in mild conditions. The use of various enzymes such as proteases is widely practiced in the industry, yet there are various limitations as it is of high cost and there is a limited availability of food-grade enzymes in the market. Moreover, high-throughput purification and the identification analysis of these peptides are currently being studied to further understand the functionality and characterization of the bioactive peptides. This review mainly focuses on the novel bioactive peptides derived from fish protein hydrolysates from various fish wastes and byproducts. The hydrolysis conditions, source of hydrolysate, and amino acid sequence of these novel peptides are presented, along with their corresponding methods of analysis in purification and identification. The use of various enzymes yields novel peptides with potent bioactivities, such as antiproliferative, antimicrobial, antihypertensive, antiglycemic, antitumor, and antioxidative biological functions. The increasing interest in proteomics in marine and aquatic waste utilization continues due to these products’ bioactivity and sustainability. Full article