•The use of HP-UAE as a strategy to intensify extraction is still incipient.•The latest trends and state of the art of HP-UAE extraction processes are detailed.•The influence of physical and medium ...parameters on the HP-UAE processes was discussed.•The main applications of HP-UAE, mostly in the last ten years, were presented.•The scale of application and the main mathematical models were discussed.
Natural products are a source of a wide range of chemical compounds, from pigments to bioactive compounds, which can be extracted and used in different applications. Due to consumer awareness, the interest in natural compounds significantly increased in the last decades, prompting the search for more efficient and environmentally friendly extraction techniques and methods. Pressurized liquids and fluids (sub and supercritical) are being explored to extract natural compounds within the green process concept. The combination of these techniques with ultrasound has emerged as an alternative to intensify the extraction process efficiently. In this context, this work presents a comprehensive review and current insights into the use of high-pressure systems, specifically supercritical fluid extraction and pressurized liquid extraction assisted by ultrasound, as emerging technologies for extracting bioactive compounds from natural products. The extraction mechanisms, applications, and the influence of operational parameters in the process are addressed, in addition to an analysis of the main challenges to be overcome for widespread application.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
The growing interest in ingredients from natural sources has expanded the need for quality assessments of plant extracts. Analytical quality-by-design (AQbD) has been increasingly applied in ...regulated environments such as pharmaceutical industries and, more recently, for the bioactive compounds found in botanical materials. This work aimed to obtain qualitative (overall resolution and maximum peak capacity) and quantitative performances for target analytes using AQbD principles. The analytical target profile was elaborated; critical method parameters (independent variables) that affect the critical method attributes (dependent variables) were selected from a risk assessment for a reversed-phase liquid chromatography with diode array detection (RPLC-DAD) method. YMC-Triart C18 (3.0 × 100 mm, 1.9 μm) and a gradient elution using 0.2% acetic acid and methanol:acetonitrile 1:3 (v/v) were chosen as the stationary and mobile phases, respectively. The optimal and robust conditions (temperature at 33.3 °C, flow rate of 0.68 mL.min
−1
, and a gradient slope of 4.18%.min
−1
) were established by the method operable design region (MODR). The validation was performed by accuracy profiles using 90% expectation tolerance intervals for the selected compounds found in
Citrus
spp. using
C. japonica
as blank matrix. The lower limits of quantification for hesperidin, bergapten, herniarin, and citropten were 5.32, 0.40, 0.49, and 0.52 mg.L
−1
, respectively (acceptance limit was set at ± 20%). Nobiletin did not show an adequate quantitative performance.
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DOBA, EMUNI, FIS, FZAB, GEOZS, GIS, IJS, IMTLJ, IZUM, KILJ, KISLJ, MFDPS, NLZOH, NUK, OILJ, PILJ, PNG, SAZU, SBCE, SBJE, SBMB, SBNM, UILJ, UKNU, UL, UM, UPUK, VKSCE, ZAGLJ
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
•A comprehensive UPLC-PDA/UPLC-HRMS method was developed for citrus peels.•In this study, 24 phenolic compounds and 5 limonoids in lime, lemon, and rangpur lime samples were identified.•The method is ...short compared to others recently published.
In this work, a method based on ultra-high-performance liquid chromatography with a photodiode array detector (UPLC-PDA) was developed to comprehensively analyze phenolic compounds in peels of lime (Citrus × latifolia), lemon (Citrus limon), and rangpur lime (Citrus × limonia). The reverse-phase separation was achieved with a C18 fused-core column packed with the smallest particles commercially available (1.3 um). The method was successfully coupled with high-resolution mass spectrometry (HRMS), allowing the detection of 24 phenolic compounds and five limonoids in several other citrus peels species: key lime, orange and sweet orange, tangerine, and tangerine ponkan, proving the suitability for comprehensive analysis in citrus peel matrices. Additionally, the developed method was validated according to the Food and drug administration (FDA) and National Institute of Metrology Quality and Technology (INMETRO) criteria, demonstrating specificity, linearity, accuracy, and precision according to these guidelines. System suitability parameters such as resolution, tailoring, plate count were also verified.
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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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•HIUS-PLE-SPE allowed the extraction and concentration of hesperidin from an industrial waste;•The On-line HPLC-UV coupling to the extractive system opens new perspectives to the ...quantification of bio extracts in real time;•Thermal processes favored the extraction of hesperidin from lime waste;•HIUS-PLE-SPE extract presented until 10 times higher hesperidin content and antioxidant activity than extracts acquired by classic extraction techniques;•The extraction and analysis method proposed in this research is in accordance with the principles of green chemistry in the sense of using eco-friendly solvents.
Hesperidin is a phenolic compound usually found in citrus fruits, which is known for its anti-inflammatory and antioxidant properties. This bioactive compound has already been used to formulate medications to treat chronic venous insufficiency. In this work, through a system which allows the in-line coupling of the pressurized liquid extraction (PLE) and high-intensity ultrasound (HIUS) with solid phase extraction (SPE), and analysis by high-performance liquid chromatography with UV–Vis detector (HPLC-UV) in on-line mode, a method was developed to obtain, separate, and quantify hesperidin from the industrial waste of lime. An eco-friendly approach with water and ethanol as extraction solvents was used. Parameters such as temperature (80, 100, and 120 °C) and HIUS power (0, 200, and 400 W) were evaluated regarding hesperidin yield. In this context, the higher hesperidin yield (18.25 ± 1.52 mg/g) was achieved using water at a subcritical state (120 °C and 15 MPa). The adsorbent SepraTM C-18-E isolated hesperidin from the other extracted compounds employing 50% ethanol in the SPE elution. The possibility ofon-lineanalysis coupling a high-performance liquid chromatograph to an ultraviolet detector (HPLC-UV) system was studied and shown to be a feasible approach for developing integrated technologies. Conventional extractions and their antioxidant capacities were evaluated, highlighting the advantages of the HIUS-PLE-SPE extractive method. Furthermore, the on-linechromatographic analysis showed the potential of the HIUS-PLE-SPE- HPLC-UV system to quantify the extracted compounds in real time.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPCLJ, UPUK, ZAGLJ, ZRSKP
Some flavonoids identified in beet stalks can help the antioxidant endogenous defenses during a chronic inflammation process. The current study investigates the effect of polyphenols present in beet ...stalks and leaves on liver oxidative damage in mice fed a high-fat diet (HF). The control (CT) or HF diet groups were supplemented with dehydrated beet stalks and leaves (SL) or beet stalk and leaf ethanolic extract (EX). In terms of Vitexin-rhaminoside equivalents (VRE), EX groups received ~5.91 mg of VRE·100 g
diet, while the SL groups received ~3.07 mg VRE·100 g
diet. After 8 weeks, we evaluated fasting blood glucose; cholesterol, hepatic Malondialdehyde (MDA) levels and hepatic Glutathione (GSH), Glutathione peroxidase (GPx), Glutathione reductase (GR) and Superoxide dismutase (SOD) activity. Dehydrated beet stalks and leaves (HFSL) attenuated the deleterious effects of a HF diet on lipid metabolism, reduced fasting blood glucose levels, ameliorated cholesterol levels and reduced GPx and GR activities (
< 0.05) compared to the HF group. However; the addition of ethanolic extract from beet stalks and leaves was unable (
> 0.05) to prevent the liver damage caused by HF diet in mice. The presence of flavonoids, such as Vitexin derivatives in beet stalks and leaves can help the liver damage induced by HF diet.
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.
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
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