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.
A PLE-SPE extraction process for the anthocyanins from Jabuticaba wastes was developed using an eutectic mixture, this acting simultaneously as solvent and stabilizing agent.
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•Combining ethanol and water as a safe mobile phase to UPLC-analysis of anthocyanins.•Fast, green, and universal method to analyze anthocyanins.•Identification of 53 anthocyanins from ...9 foods.•The developed method achieved a high green analytical score.
This work developed a universal UPLC-PDA method based on safe reagents to analyze anthocyanins from different foods. Nine foods were studied by the developed chromatographic method, which was constructed using a solid core C18 column and a binary mobile phase composed of (A) water (0.25 molcitric acid.Lsolvent−1), and (B) ethanol. A total running time of 6 min was obtained, the faster comprehensive method for anthocyanins analysis. Mass spectrometry analysis was employed to identify a comprehensive set of 53 anthocyanins comprising glycosylated and acylated cyanidin, pelargonidin, malvidin, peonidin, petunidin, and delphinidin derivatives. Cyanidin-3-O-glucoside (m/z+ 449) and cyanidin-3-O-rutinoside (m/z+ 595) were used as standards to validate the accuracy of the developed method. The analytical parameters were evaluated, including intra-day and inter-day precision, robustness, repeatability, retention factor (k), resolution, and peak symmetry factor. The current method demonstrated excellent chromatographic resolution, making it a powerful tool for analyzing anthocyanins pigments.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
•Selective extraction obtains separate extracts of carnosic and rosmarinic acids.•No additional separation steps are needed.•Use of green, eco-friendly, bio-based solvents.•Solvent selectivity is ...maintained when employed in other extraction techniques.•UAE accelerates the extraction of primary phenolic acids from rosemary.
Carnosic (CA) and rosmarinic (RA) acids are the primary phenolic acids in hydrophilic rosemary extracts. Their combination exhibits high antioxidant activity and can be explored in several applications. This study aimed to develop an extraction procedure using bio-based solvents to recover two rosemary extracts, one rich in CA and the other in RA. By using ultrasound-assisted extraction (UAE) and a pool of 34 solvents, we evaluated nominal power (W), extraction time (min), and solvent water percentage (% H2O) regarding yield and selectivity. The authors propose a sequential UAE procedure validated by applying ethanol 99.5 % (v/v), 240 W, and 5 min to recover a rich fraction of 24.0 mgCA.gbiomass−1; followed by a second step using AmAc:LA (1:2 M ratio), 20 % H2O (m/m), 320 W, and 5 min that resulted in 8.4 mgRA.gbiomass−1. Our results indicate that modulating the solvent composition and process temperature is critical to increasing extraction yields and selectivity.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
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•A new UHPLC-PDA-MS/MS method to assess quality control from propolis.•Adulteration in Brazilian commercial propolis samples.•The dangerous situation regarding the commercialization ...of propolis extracts.•35% of propolis extracts have not met the minimum criteria for commercialization.
Propolis is a rich source of known and largely explored bioactive compounds with many pharmacological properties. It is used in several commercialized products, such as propolis-enriched honey, candies, mouth and throat sprays, soaps, toothpaste, and skin creams. However, the great diversity of propolis products and different types make the standardization of realistic quality control procedures challenging. Moreover, the extraction of propolis bioactive compounds depends on the technique and the solvent used. In Brazil, the Ministry of Agriculture, Livestock, and Supply (MAPA) set standards to establish commercialized propolis extracts' identity and quality. In addition, according to legislation, propolis extracts must present the main classes of phenols at 200 and 400 nm on the UV spectrum. Still, it is not specified which analysis method should be used to guarantee feasible quality control of the commercialized samples. For this, we proposed a new fast UHPLC-PDA-MS/MS method for analysis and quantification of propolis phenolic compounds. Moreover, we hypothesize that there is no efficient monitoring regarding the quality of the propolis extracts sold in Brazilian stores. Therefore, the present study aimed to perform quality control of 17 Brazilian propolis extracts produced in the Southeast region (green or brown – the most representative samples). The dry extract content (% g/mL), oxidation index (seconds), total flavonoids, and phenolics (% m/m) of each sample were compared with legislation. We conclude that using the UHPLC-PDA method and the investigation that allowed the comparison with the current legislation efficiently practical problems in the commercialization of propolis extracts. However, of the 17 analyzed samples, 6 did not meet the desired the recognized standards, denoting a lack of supervision and efficient quality control, which highlights a dangerous situation regarding the commercialization of this critical product used in several industrial fields, mainly in the food and pharmaceutical sector.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
Analyzing compounds such as polyphenols in solid samples frequently uses a solid-liquid extraction step. The solid-liquid extraction and analysis integration in a single equipment is not commercially ...available since several challenges are inherent to this hybridization. In the context of developing more sustainable analytical procedures, innovative techniques are demanded. Given that, this work proposes a new integrative system (2D PLE × HPLC-PDA) and presents its validation for bioactive compound extraction and online quantification, discussing the main advantages and cares that need to be taken. Two food byproducts – passion fruit bagasse and coffee husks – were chosen as solid model samples. The system was configured to perform pressurized liquid extraction (PLE) with periodical automated extract injection in the HPLC, consequently obtaining the online quantification of target compounds from the solid samples. In parallel with the online injections, extract fractions were collected and submitted to offline analysis in which the extraction yield of piceatannol and chlorogenic acid and caffeine were evaluated, respectively, for passion fruit bagasse and coffee husks. The extraction yields obtained by online and offline injections were compared and were significantly equal (p > 0.05). Thus, the 2D PLE × HPLC-PDA system represents a feasible tool to integrate solid sample preparation and chemical analysis of biocompounds in a single and online step.
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•An automated system to analyze bioactive compounds from solid samples is presented.•2D PLE × HPLC-PDA system integrates sample preparation online with chromatography.•The system validation compares online and offline extract quantification.•The new online method reports significantly equal yields with offline quantification.•The online method represents a feasible tool for analyzing bioactive compounds.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
This study delves into an innovative biorefinery approach to extract multiple high-value compounds from a single biomass source, Halobacterium salinarum R1, a resilient halophilic microorganism. By ...using bio-based solvents, namely an aqueous solution of gamma-valerolactone (GVL) and ethanol, a simple and efficient pipeline approach was developed, recovering unique pigments, including C 50 bacterioruberin, as well as two additional fractions consisting of protein and polysaccharides. The process is based on sustainable engineering and green chemistry principles, providing a viable alternative to replacing non-renewable solvents. The study addresses environmental concerns by employing bio-based solvents while presenting a cost-effective and sustainable solution. This approach contributes to developing a high-performance and sustainable alternative, promoting the development of a blue bioeconomy.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
Propolis is a bee product with a complex chemical composition formed by several species from different geographical origins. The complex propolis composition requires an accurate and reproducible ...characterization of samples to standardize the quality of the material sold to consumers. This work developed an ultra‐high‐performance liquid chromatography with a photodiode array detector method to analyze propolis phenolic compounds based on the two key propolis biomarkers, Artepillin C and p‐Coumaric acid. This choice was made due to the complexity of the sample with the presence of several compounds. The optimized method was hyphenated with mass spectrometry detection allowing the detection of 23 different compounds. A step‐by‐step strategy was used to optimize temperature, flow rate, mobile phase composition, and re‐equilibration time. Reverse‐phase separation was achieved with a C18 fused‐core column packed with the commercially available smallest particles (1.3 nm). Using a fused‐core column with ultra‐high‐performance liquid chromatography allows highly efficient, sensitive, accurate, and reproducible determination of compounds extracted from propolis with an outstanding sample throughput and resolution. Optimized conditions permitted the separation of the compounds in 5.50 min with a total analysis time (sample‐to‐sample) of 6.50 min.
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BFBNIB, FZAB, GIS, IJS, KILJ, NLZOH, NUK, OILJ, SAZU, SBCE, SBMB, UL, UM, UPUK
Rosemary and sage are composed of bioactive molecules in high demand by the food, pharmaceutical, and cosmetic industries to produce value-added products. After the industrial extraction of essential ...oils, the raw material still has nonvolatile compounds interesting for other commercial products. The nonvolatile fraction comprises terpenes and phenolic acids (rosmarinic acid, carnosic acid, and derivatives), which are economically valuable. Modern extraction techniques integrated with other processes within the biorefinery are highly needed to obtain well-evaluated products from these plant matrices.
The chemical and biological features of such compounds from rosemary and sage were reviewed and deeply discussed. Recovery technologies, including the influence of operational parameters on extract yield and concentration, were addressed in the past 20 years of available literature. Critical issues for modern production systems, such as applying emerging solvents and developing platforms for zero-waste biorefineries, were also highlighted.
The bioactive compounds of rosemary and sage stand out for their specific biological properties. This feature allows obtaining well-defined extracts through modern and emerging extraction technologies, enabling higher specificity for industrial applications. Both raw materials are attractive for biorefineries with current production concepts. However, complete studies addressing the biorefinery of these herbs from a technical, scalable, economic, and environmental point of view are still needed.
•Rosemary and sage are promising to be used in biorefinery towards the zero-waste concept.•Non-volatile fraction from rosemary and sage display attractive biological properties.•Phenolic acids and diterpenes rich extract plays target roles as a functional food ingredient.•Modern techniques can modulate the extraction to produce single well-defined extracts.•New process platforms for both matrices are still needed, targeting lab-to-industry scales.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
•Valorization of grape pomace by extracting natural pigments.•A new sustainable and economically feasible process for extracting anthocyanins.•Nicotinamide-based eutectic mixture was used to recover ...anthocyanins.•Stabilizing anthocyanins in SiO2 material approved in food and pharmaceutical sector.•Obtaining high-purity and thermal stable anthocyanins.
Concentrated in the skins of red grapes are the anthocyanins, the primary colorants responsible for the fruits' reddish-purple color. These colorants are recognized for their significant antioxidant properties and potent nutraceutical and pharmaceutical ingredients. Nevertheless, their widespread use is compromised by the (i) need for more efficient yet sustainable downstream processes for their recovery and (ii) by the challenges imposed by their poor stability. In this work, these drawbacks were overcome by applying eutectic solvents and stabilizing agents. Besides, the anthocyanins were successfully loaded into a solid host material (approved in both food and pharmaceutical sectors) based on silicon dioxide (SiO2, loading capacity: 1extract:7silica m/m). Summing up, with the process developed, the extraction yield (21 mganthocyanins.gbiomass−1) and the stability (under 55, 75, and 95 °C) of the recovered anthocyanins were over three times better than with the conventional process. Finally, the raw materials and solvents were recycled, allowing an economical and environmentally friendly downstream process.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
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•Highlighting a new green extraction platform for the valorization of grape pomace;•Investigating the techno-economic analysis of a eutectic solvent extraction approach;•Exploring the ...potential of alternative extraction processes based on DES in the industrial sector;•Discussing process design integration for DES recycling.
A techno-economic analysis of a novel eutectic solvent-based platform useful to recover anthocyanins from grape pomace was performed. The study addressed the economic impact of conventional drying methods and explored the economic implications of purification strategies to separate the extract from the eutectic solvent. This was exemplified by employing solid-phase extraction (SPE) with C18-based adsorbent material. An alternative low-energy demanding approach using SiO2 particles was also assessed for profitability as a freeze-drying replacement strategy. The results highlighted challenges in the economic feasibility of eutectic solvent reusability when conventional SPE is applied, highlighting the need to obtain new and inexpensive bio-based adsorbents. Moreover, it was uncovered that the SiO2-based drying strategy presents itself as a financially viable alternative, effectively addressing the elevated energy requirements associated with conventional drying methods. The findings highlight the potential of alternative solvents-based processes, particularly towards challenges related to the circularity of raw materials.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
