Supercritical Fluid Extraction Research Articles

Optimizing Green Extraction Methods for Maximizing the Biological Potential of Dandelion, Milk Thistle, and Chamomile Seed Extracts

This study investigates the underutilized potential of agri-crops from the Asteraceae family by employing sustainable and green technologies (supercritical fluid, ultrasound, and Soxhlet extractions) to enhance the recovery of bioactive compounds. A total of 21 extracts from native and waste seeds of dandelion, milk thistle, and chamomile were systematically compared utilizing a combination of solvents (supercritical CO2 and absolute or aqueous ethanol). Supercritical CO2 extraction yielded up to 281 mg/g of oils from native seeds, while conventional techniques with ethanol recovered an additional 142 mg/g of extracts from waste seeds. Notably, waste seed extracts exhibited superior biological activity, including potent antioxidant properties (IC50 values as low as 0.3 mg/mL in the DPPH assay) and broad-spectrum antimicrobial activity against 32 microbial strains, including methicillin-resistant Staphylococcus aureus, Gram-negative bacteria, and yeast strains. Phenolic compounds were abundant, with up to 2126 mg GAE/g, alongside 25.9 mg QE/g flavonoids, and 805.5 mg/kg chlorophyll A. A selective anticancer activity of waste milk thistle extracts was observed, with a selectivity index of 1.9 to 2.7. The oils recovered from native seeds demonstrated lower bioactivity and are well-suited for applications in food. The potent bioactivity of the smaller quantities of waste seed extracts positions them as valuable candidates for pharmaceutical use.

A Descriptive Analysis of the Nutraceutical Constituents, Extraction Techniques, and Possible Health Benefits of Tamarind

Background: Tamarind is a multifunctional tree, with nearly every portion having significant nutritional or therapeutic use. The fruit, which produces acidic pulp, is the most valuable and often utilized portion. Objective: The aim of this paper is to discuss the distribution, habitat, chemical constituents and extraction techniques of tamarind. Methods: This study reviews the chemical constituents, health benefits and extraction techniques of tamarind. Databases such as PubMed, Scopus, Science Direct, and Google Scholar were used to search articles from 1990 to 2022. The key search terms included tamarind, phytoconstituents extraction and anti-nutritional factor. Research studies also included similar plant parts extracted from similar solvents which were considered in this review. Results: According to our observations, Tamarindus indica is a crucial plant with significant pharmacological properties. It is extensively used as a conventional medicine to treat a variety of disorders; however, its active ingredients require further investigation for future drug development and pharmacological activity. Tamarind contains a diverse range of bioactive compounds, including polyphenols, flavonoids, alkaloids, vitamins, and minerals, which have been associated with various health-promoting properties. The study examines different extraction methods used to isolate tamarind's bioactive constituents, such as solvent extraction, supercritical fluid extraction (SFE), and microwave-assisted extraction (MAE). Furthermore, the research highlights the potential health benefits of tamarind, including antioxidant activity, anti-inflammatory effects, gastrointestinal support, cardiovascular benefits, and antimicrobial properties. Discussion: Tamarind includes citric acid, linoleic acid, volatile oils, vitamin C, potassium, Camp sterol, -amyrin, Tannins, saponins, and glycosides as a result of this. It has several pharmacological properties such as reducing swelling, preventing oxidation, hypolipidemic, weight loss, antibacterial, hepatoprotective, anthelmintic, and painkiller properties. These properties will assist to generate interest in Tamarind and develop novel preparations with more medicinal and commercial potential. The findings indicate that tamarind holds significant promise as a natural resource for developing functional foods, nutraceuticals, and pharmaceuticals with potential positive impacts on human health.

Green synthesis of silver nanoparticles from supercritical CO2 mediated Lagerstroemia speciosa extract: Characterization, antimicrobial and antibiofilm activity

In the current study, optimal supercritical fluid extract (SFE) of Lagerstroemia speciosa (LS) leaves at pressure 29.59 megapascal (MPa), temperature 89.50 ºC and extraction time 53.85 min. was used to extract phenolic compounds for the synthesis of silver nanoparticles (AgNPs). The synthesis was studied for 0-20 hrs. Initially the synthesis of nanoparticles (SFELS-AgNPs) was confirmed using UV -spectroscopy. It demonstrated a maximum surface plasmon resonance at 430 nm. The crystallite dimension of nanoparticles was determined using X-ray diffraction (XRD) (13.47 nm), Transmission electron microscopy (TEM), zeta potential analysis and energy-dispersive X-ray analysis (EDAX) were used to analyze the morphology, surface charge and presence of differential elements in SFELS-AgNPs respectively. Developed nanoparticles revealed antimicrobial activity against two gram-positive viz. Staphylococcus aureus and Bacillus cereus, and three gram-negative bacteria viz. Klebsiella pneumonia, Pseudomonas aeruginosa and Escherichia coli. The nanoparticle showed a minimum inhibitory concentration (MIC) of 64 μg/ml whereas the minimum bactericidal concentration (MBC) 128 μg/ml against K. pneumonia. They significantly inhibited K. pneumonia biofilm formation which was confirmed using scanning electron microscopy (SEM). The results were encouraging compared to the standards drug Chloramphenicol and other controls. The generated nanoparticles have highly effective antimicrobial properties against pathogenic bacteria.

Supercritical fluid extraction prior pulsed electric fields to improve high-added-value compounds recovery from salmon side streams: Evaluation of protein, bioactive peptides and minerals

A sequential extraction process combining supercritical fluid extraction (SFE: 25.0 MPa, 75 min, 50.0 °C, and 10.0 mL/min flow) with pulsed electric fields (PEF: 3.0 kV/cm, 300 kJ/kg for head/backbones, 124.8 kJ/kg for viscera) or conventional extraction (CE: 60 min, 300 rpm) was optimized to enhance the recovery of high-added-value compounds, including proteins, bioactive peptides, minerals, heavy metals, and total antioxidant capacity (TAC) from salmon side streams. Protein levels increased notably with PEF, particularly in viscera liquid extracts, reaching 15.5 g/100 g. Bioactive peptides displayed anti-inflammatory, immunomodulatory, anticancer, hypolipidemic, and antithrombotic potential. Viscera liquid extracts showed high TAC (402.8 and 3263.6 μM). ICP-MS analysis revealed PEF treatment helps solid matrices retaining more minerals and heavy metals. Principal component analysis (PCA) on proteins, peptides, minerals, and heavy metals elucidated PEF's impact, identifying two main components affecting the salmon matrix and extract composition.

The use of green technologies for processing lupin seeds (Lupinus angustifolius L.): Extraction of non-polar and polar compounds for concentrated-protein flour production

This study aimed to promote the valorization of lupin seeds by extracting both non-polar and polar fractions to produce a protein-rich flour suitable for food applications. Green extraction methods such as Supercritical Fluid Extraction (SFE) and SFE followed by gas-expanded liquid extraction with ethanol/CO2 mixtures were employed. SFE yielded lupin oil with extraction yields ranging from 2.27 ± 0.02 to 4.5 ± 0.2 %, significantly influenced by temperature (40 and 60 °C) and pressure (150–350 bar). SFE extracts exhibited higher tocopherol concentration, particularly α-tocopherol (116.7–296.9 µg/g oil) and γ-tocopherol (2006–4749 µg/g oil), compared to the Bligh and Dyer (B&D) method. The fatty acid profiles were similar, although they differed slightly in composition, with the extracts obtained by SFE having higher proportions of unsaturated fatty acids (UFA) and lower proportions of saturated fatty acids (SFA). Ethanol proportion positively correlated with extraction yield (r = 0.991), resulting in higher recovery of polar lipids (PL). However, increasing ethanol percentage decreased the phenolic compounds content and antioxidant activity assessed by DPPH radical scavenging method. SFE produced lupin flour with 36 % protein content, increased by 11 % post-extraction. Ethanolic extraction also increased protein concentration, albeit less pronounced (6.8–11 % increase post-sequential extraction). Essential amino acids consistently increased post-SFE, highlighting the potential of this sustainable method to yield protein-rich flour free of non-GRAS (Generally Recognized as Safe) solvents and containing compounds essential for human health. SDS-PAGE analysis showed consistent protein profiles across all extracted flours, while FTIR assessment revealed changes in the secondary structure of proteins induced by SFE and SFE followed by gas-expanded liquid extraction processes. These findings highlight the potential of this approach to enhance the nutritional and commercial value of lupin-based products while promoting sustainable food processing practices.

Comprehensive analysis of oils and remaining solid matrices from supercritical fluid extraction of salmon side streams: Fatty acids, bioactive peptides, minerals, and heavy metals

Atlantic salmon (Salmo salar) side streams (head, backbone, and viscera) are nutrient-rich and offer potential for valorization. This study evaluates supercritical fluid extraction (SFE) and solvent extraction (SE) methods for recovering oils, fatty acids, bioactive peptides, minerals, heavy metals, and antioxidants from these byproducts. Both the oil and the remaining solid resulting from the extraction process were analyzed. SFE was more effective in extracting fatty acids from heads and backbones. However, SE yielded a higher peptide content, with SE backbone solids containing 281 peptides, and SE viscera and heads containing 220 peptides each. In contrast, SFE-derived solids had significantly fewer peptides: 9 in heads, 129 in backbones, and 130 in viscera. The identified peptides exhibit potential functional properties, including antioxidant, anti-inflammatory, antithrombotic, immunomodulating, anticancer, and hypolipidemic effects. Mineral and heavy metal content in all extracts met safety standards. SFE-derived matrices had the highest calcium levels (49.7 mg/g in heads, 24.2 mg/g in backbones) and lower heavy metal concentrations than SE. Arsenic, cadmium, mercury, and lead levels were 1.8 mg/kg, 1.8 μg/kg, 55.0 μg/kg, and 25.7 μg/kg, respectively, for SFE, compared to SE's higher values (e.g., 3.5 mg/kg for arsenic). Both methods produced extracts with promising antioxidant activity.

Nontarget analysis of natural flavor metabolites in tobacco extracts

Large-scale production of tobacco generates significant amounts of waste, making the reuse and recycling of tobacco waste crucial for sustainability. However, the high diversity of tobacco metabolites requires a comprehensive analysis of tobacco waste extracts, so as to optimize extraction selectivity and recovery. In this study, we thoroughly analyzed the metabolic composition of 168 tobacco extracts using nontarget analysis. The extracts were derived from 56 tobacco wastes covering all four major tobacco types: flue-cured, dark air-cured, Burley, and Oriental tobaccos. From each sample, we obtained three types of extracts, such as concretes, absolutes, and supercritical fluid extraction (SFE) oils, through various extraction protocols. By matching deconvolved experimental MS/MS spectra with databases, 587 metabolites were putatively annotated, which were categorized into 24 groups, including alkaloids, indoles, and flavor compounds. The metabolic compositions of extracts from dark air-cured and Burley tobaccos were found to be similar, whereas flue-cured and Oriental tobaccos contained more diverse flavor components. Notably, concretes of various tobaccos prepared with 70 %-ethanol contained similar amounts of addictive alkaloids. However, the absolutes obtained by sequential extraction of these concretes with 95 %-ethanol effectively removed alkaloids while modestly maintaining the flavor compounds. Conversely, extraction protocols incorporating supercritical fluid extraction followed by 95 %-ethanol extraction resulted in the loss of most flavor compounds, likely due to the incompatibility between the solvents used in the two extraction steps. In conclusion, our study demonstrates that absolutes derived through secondary extraction with varying ethanol-water ratios holds significant potential for utilization.

Recovery of bioactive compounds from pineapple waste through high-pressure technologies

This study aimed to obtain bioactive compounds from the residue from pineapple (Ananas comosus L. Merril) juice processing, using supercritical fluid extraction (SFE) and pressurized liquid extraction (PLE). The SFE were performed using ethanol as a co-solvent and evaluating different pressure, temperature, and co-solvent percentage. For the PLE, temperature and ethanol percentage were assessed. The best extraction conditions for SFE were 20 MPa, 60 °C, and 15 % ethanol, while for PLE they were obtained at 10 MPa, 100 °C with 50 % and 75 % ethanol. Both methods presented a higher concentration of bioactives than other recognized vegetable waste sources. However, it was observed that PLE showed a higher overall extract yield, phenolic compounds, flavonoids, carotenoids, and antioxidant activity. The main phenolic compounds identified were caffeic acid and ferulic acid. Therefore, pineapple residue is a potential source of bioactive compounds, and the pressurized liquid extraction technique proved more efficient for their recovery.

Co-solvent assisted supercritical fluid extraction of Curcuma caesia Roxb. (black turmeric) as a green and sustainable technology: Its bioactivity and anti-cancer properties

This study investigates a green method to extract black turmeric oleoresin (BTO) using supercritical fluid extraction (SFE) with ethanol as co-solvent. The optimized parameters of SFE were 350 bar/65 °C/150 min, yielding 6.56 g oleoresin/100 g dwb and 134 μg total curcuminoids/ g dwb (dry weight basis). The conventional ethanol extraction gave 13.94 g/100 g oleoresin, and the total curcuminoids in the oleoresin was 128 µg/g dwb. Hence ethanol was used as a co-solvent and this approach increased the yield of the oleoresin to 12.53 g/100 g and curcuminoids (223 µg/g) among all the methods. The SFE+ co-solvent extracted BTO showed significant antioxidant activity. Phytochemicals present in extracted oleoresin were quantified using HPLC, LCHRMS, GCMS, and FTIR. Similarly, a comparatively higher (84 %) anti-inflammatory activity compared to diclofenac and bactericidal effects against Salmonella typhi, Pseudomonas aeruginosa and Listeria monocytogenes have been observed. The remarkable in vitro anticancer activity of the extract in HepG2 (IC50: 6 µL/mL) and HPAC (IC50: 5 µL/mL) cell lines indicated the potency of the extract.

Carbon Dot Micelles Synthesized from Leek Seeds in Applications for Cobalt (II) Sensing, Metal Ion Removal, and Cancer Therapy.

Popular photoluminescent (PL) nanomaterials, such as carbon dots, have attracted substantial attention from scientists due to their photophysical properties, biocompatibility, low cost, and diverse applicability. Carbon dots have been used in sensors, cell imaging, and cancer therapy. Leek seeds with anticancer, antimicrobial, and antioxidant functions serve as traditional Chinese medicine. However, leek seeds have not been studied as a precursor of carbon dots. In this study, leek seeds underwent a supercritical fluid extraction process. Leek seed extract was obtained and then carbonized using a dry heating method, followed by hydrolysis to form carbon dot micelles (CD-micelles). CD-micelles exhibited analyte-induced PL quenching against Co2+ through the static quenching mechanism, with the formation of self-assembled Co2+-CD-micelle sphere particles. In addition, CD-micelles extracted metal ion through liquid-liquid extraction, with removal efficiencies of >90% for Pb2+, Al3+, Fe3+, Cr3+, Pd2+, and Au3+. Moreover, CD-micelles exhibited ABTS•+ radical scavenging ability and cytotoxicity for cisplatin-resistant lung cancer cells. CD-micelles killed cisplatin-resistant small-cell lung cancer cells in a dose-dependent manner with a cancer cell survival rate down to 12.8 ± 4.2%, with a similar treatment function to that of cisplatin. Consequently, CD-micelles functionalized as novel antioxidants show great potential as anticancer nanodrugs in cancer treatment.

Volatiles extracted from Melaleuca Rugulosa (Link) Craven leaves: comparative profiling, bioactivity screening, and metabolomic analysis

BackgroundMelaleuca species (family Myrtaceae) are characterized by their wide-ranging applications as antimicrobials and in skin-related conditions. Herein, we estimated the volatile profile and biological significance of M. rugulosa (Link) leaves for the first time supported by a dereplication protocol.Materials and methodsVolatile components were extracted using hydrodistillation (HD), supercritical fluid (SF), and headspace (HS) techniques and identified using GC/MS. The variations among the three extracts were assessed using principal component analysis and orthogonal partial least square discriminant analysis (OPLS-DA). The extracted volatiles were tested for radical scavenging activity, anti-aging, and anti-hyperpigmentation potential. Finally, disc diffusion and broth microdilution assays were implemented to explore the antibacterial capacity against Streptococcus pyogenes, Staphylococcus aureus, Clostridium perfringens, and Pseudomonas aeruginosa.ResultsThe yield of the SF technique (0.8%) was three times higher than HD. GC/MS analysis revealed that the oxygenated compounds are the most proponents in the three extracts being 95.93% (HD), 80.94% (HS), and 48.4% (SF). Moreover, eucalyptol (1,8-cineol) represents the major component in the HD-EO (89.60%) and HS (73.13%) volatiles, while dl-α-tocopherol (16.27%) and α-terpineol (11.89%) represent the highest percentage in SF extract. Regarding the bioactivity profile, the HD-EO and SF-extract showed antioxidant potential in terms of oxygen radical absorbance capacity, and β- carotene assays, while exerting weak activity towards DPPH. In addition, they displayed potent anti-elastase and moderate anti-collagenase activities. The HD-EO exhibited potent anti-tyrosinase activity, while the SF extract showed a moderate level compared to tested controls. OPLS-DA and dereplication studies predicted that the selective antibacterial activity of HD-EO to S. aureus was related to eucalyptol, while SF extract to C. perfringens was related to α-tocopherol.ConclusionsM. rugulosa leaves are considered a vital source of bioactive volatile components that are promoted for controlling skin aging and infection. However, further safety and clinical studies are recommended.

Optimization of Supercritical Fluid Extraction of Rare Earth Elements from Complex Ores Using a Tributyl Phosphate-Nitric Acid Adduct

Optimization of Supercritical Fluid Extraction of Rare Earth Elements from Complex Ores Using a Tributyl Phosphate-Nitric Acid Adduct

Araçaúna (Psidium myrtoides) flour: Sequential extraction with supercritical carbon dioxide and pressurized fluids

Araçaúna (Psidium myrtoides) is a native fruit from the Brazilian Atlantic Forest. It was studied for the proximate composition of its flour and sequential extraction using supercritical fluid extraction (SFE) in the first stage with CO2 and pressurized liquid extraction (PLE) with ethanol and water in the second and third stages, respectively, at 50°C and 60°C. The proximate analysis revealed essential information about the flour regarding the content of protein, carbohydrates, lipid, ash and moisture. The sequential extraction at 60°C resulted in high yields (42.22 %). The first stage using SFE captured the volatile fraction, notably 1,4-diethylbenzene, which corresponds to 53.70 % of the total volatile compounds identified in the araçaúna. Comparing the second and third stages, the third stage with water at 50°C produced the highest levels of phenolic compounds (33.06±2.26 mg GAE/g extract), total monomeric anthocyanins (3.91±2.10 mg C3G/g extract), antioxidant activity by ORAC (415.13±13.66 µmol TE/g extract) and FRAP (747.16±18.49 µmol TE/g extract), and cyanidin-3-glucoside as the predominant compound (4.83 % w/w).

Optimization of Supercritical Extraction of Cannabidiol Using Response Surface Methodology

Hemp, also known as Cannabis sativa L., contains over 80 cannabinoids, with cannabidiol (CBD) being the primary neuroactive component. CBD possesses various pharmacological properties and is considered a non-psychoactive compound, making it a promising component for various applications, such as pharmaceuticals, cosmetics, and nutraceuticals. The aim of this study was to identify the optimal conditions for extracting CBD from hemp using supercritical fluid extraction (SFE). Response surface methodology (RSM) was employed to optimize the SFE conditions. The Box–Behnken design and the central composite design were utilized to refine the extraction parameters, including extraction time, temperature, and pressure. The statistical significance and reliability of the optimized conditions were confirmed by the significant influence of these independent variables on CBD yield. The extracted CBD was purified to a high level of purity and converted from cannabidiolic acid (CBDA) through heat treatment and then analyzed using high-performance liquid chromatography (HPLC). The following extraction conditions were considered optimal and led to a CBD yield of approximately 70.46 g/kg: pressure of 48.3 MPa, temperature of 60 °C, and extraction time of 109.2 min. Validation experiments confirmed the accuracy of the model, with experimental values closely matching the predicted values (69.93 ± 0.88 g/kg). This study demonstrates that SFE is an efficient method for obtaining high-purity CBD from hemp, highlighting its potential for industrial applications. The findings suggest that optimizing SFE conditions through RSM can significantly enhance the efficiency and yield of CBD extraction, providing a robust framework for industrial-scale production.

Functions of a Complex Variable with a Large Parameter and Construction of Regions

The paper describes an experimental setup for studying the solubility of substances in SCF media and the implementation of a supercritical fluid extraction process using a pure and modified polar solvent additive. The advantages and disadvantages of this installation are analyzed, ways of improving it are indicated, leading to achieving a more accurate GFR flow rate, maintaining the necessary constant pressure in the first extract collector for fractionation of a certain component of the mixture and eliminating multiple regulation of the GFR flow rate.

Enhancement of antioxidant properties of Eisenia bicyclis extracts through combination of green extractions: Parameter optimization and comparison

We compared and optimized combined green extraction (CGE) technologies to maximize the antioxidant activity of Eisenia bicyclis through response surface methodology (RSM). Firstly, conventional extraction (CE), microwave assisted extraction (MAE), and supercritical fluid extraction by carbon dioxide (SFE-CO2) were applied to extract and compare antioxidant activities of E. bicyclis. The antioxidant activity results indicated that MAE and SFE-CO2 were superior to CE alone. Based on the optimum conditions for MAE and SFE-CO2, ultrasound-assisted extraction (UAE) and high-pressure processing (HPP) were combining to increase antioxidant activity. SFE-CO2+UAE was selected as the optimum CGE technology. The DPPH-radical scavenging activity and the total phenolic content of E. bicyclis extracts using SFE-CO2+UAE were approximately 2 and 5-fold higher than those of extracts using CE with almost 9-fold higher dieckol content. We demonstrated that E. bicyclis has substantial potential as a natural antioxidant and that CGE is more effective than CE and GE in enhancing antioxidant yields.

Anti-Inflammatory Effects and Metabolomic Analysis of Ilex Rotunda Extracted by Supercritical Fluid Extraction.

Ilex rotunda is a famous medicinal plant with many ethnopharmacological uses. It is traditionally employed for treating inflammation and cardiovascular diseases. In this study, we established green technology to extract the leaves and twigs of I. rotunda. The obtained extracts and their fractions were evaluated for their anti-inflammatory potential. In cytokine assays, the extract, n-hexane (H), methylene chloride (MC), and EtOAc (E) fractions of the twigs of I. rotunda significantly inhibited lipopolysaccharide (LPS)-induced nitric oxide (NO), interleukin (IL)-6, and tumor necrosis factor (TNF)-α production in RAW264.7 macrophages. Furthermore, the extract, H, and MC fractions of the leaves of I. rotunda modulated cytokine expression by downregulating LPS-induced NO, IL-6, and TNF-α production in RAW264.7 macrophages. Western blotting analysis revealed that the extracts and fractions of the leaves and twigs of I. rotunda inhibited inflammatory cytokines by inactivating nuclear factor kappa B (NFκB) action by reducing the phosphorylation of transcript factor (p65) and nuclear factor-kappa B inhibitor alpha (IκBα) degradation, or by inactivating mitogen-activated protein kinase (MAPK) through the p38 or ERK signaling pathways via the active ingredients of the leaves and twigs of I. rotunda. Ultra-high-resolution liquid chromatography-Orbitrap mass analysis (UHPLC-ESI-Orbitrap-MS/MS)-based molecular networking, in cooperation with social open platform-guided isolation and dereplication, led to the identification of metabolites in this plant. Our findings indicate that the leaves and twigs of I. rotunda could be promising candidates for developing therapeutic strategies to treat anti-inflammatory diseases.

Maximizing the Hesperidin Extraction Using Supercritical Carbon Dioxide and Ethanol: Theoretical Prediction and Experimental Results

Agroindustrial waste can be valorized towards the obtaining of several products such as pigments, proteins, fibers, and polyphenolic compounds with antioxidant capacity. Orange peel waste is a promising source of polyphenolic compounds such as hesperidin. However, conventional extraction techniques present some environmental limitations such as high solvent consumption and high wastewater generation. Supercritical fluid extraction (SFE) has emerged as a green extraction technique due to the low use of solvent. The aim of this study was to maximize the hesperidin extraction based on theoretical predictions of the operating conditions from empirical thermodynamic models using SFE with carbon dioxide (CO2) as a solvent. The theoretical conditions were validated experimentally on a semi-pilot scale. The extracts were evaluated in terms of hesperidin content, total polyphenol content, and antioxidant capacity. Thermodynamic prediction of the operating conditions showed that the ethanol used as a co-solvent promotes hesperidin extraction. The optimum operating conditions were 25 °C, 80 bar, and a volumetric co-solvent concentration of 10%. The validation of the operating conditions resulted in a final hesperidin concentration of 11.5 ± 0.03 g/kg of orange peel waste. The experimental results were 30.26-times higher using 10% vol of ethanol than the extraction of hesperidin with pure ethanol as a co-solvent. The total polyphenol content and antioxidant capacity resulted in 831.92 ± 40.01 mg Galic acid/100 g orange peel waste, 15.41± 0.91 EC50/mL, and 5.31 ± 0.67 µMolTrox/100 g orange peel. Finally, the prediction of operating conditions from empirical thermodynamic models such as the Peng–Robinson equation of state with some modifications (Stryjek Vera) for solid–gas equilibrium solubility calculations, allows for maximizing the content of the polyphenolic compounds using SFE.

Impact of green techniques on intricate cell wall structure of bee pollen to enhance functional characteristics and improve its in vitro digestibility.

Bee pollen is a nutrient-rich super food, but its rigid dual-layered structure limits nutrient release and absorption. The outer exine, composed of stress-resistant sporopollenin, and the inner intine, consisting of cellulose and pectin, form a barrier to digestive breakdown. This study investigates the potential of green techniques, specifically supercritical fluid extraction and ultrasonication, to disaggregate pollen cell walls, enhancing its bioavailability and maximizing nutrient utilization. Ultrasonication treated pollen (USTP) and supercritical fluid extraction-treated pollen (STP) demonstrated disruption, as evidenced by scanning electron microscopy imaging. In relation to scanning electron microscopy, techno-functional, antioxidant, and compositional analysis displayed a positive outcome, with crude lipid, protein, antioxidant activity (2,2-diphenyl-1-picrylhydrazyl activity and 2,2'-azino-bis-3-ethylbenzthiazoline-6-sulphonic acid assay) and total phenolic content increased by 34.80%, 32.58%, 10.80%, 11.37%, and 83.94%, respectively. Based on the above properties, USTP for 4 h and STP at 400 bar for 40 min were identified as the optimal conditions for disintegration. Furthermore, optimized samples analyzed for amino acid and mineral release revealed a notable increase in composition of essential amino acid and minerals (Ca, Cu, Fe, etc.) by ∼1.5 and 1.2 times, respectively. Along with significant changes in composition, fractured pollen exhibited 1.4 folds increase in protein digestibility with minor differences in thermal stability, and crystallinity as established by differential scanning calorimetry, and X-ray diffraction analysis. The study confirms that nutrient release and absorption remain restricted without pre-treatment, highlighting the necessity of specific treatment to disintegrate bee pollen before its use as a functional food ingredient. PRACTICAL APPLICATION: Bee pollen is a rich source of all the essential nutrients required by the humans and recognised as a complete food. However, its tough cellular structure restricts its utilisation in numerous food applications. Therefore, to disintegrate bee pollen and release its nutrients, ultrasonication and super critical fluid extraction processes were employed to improve its utilization for human purposes. Both the treatment techniques, enhanced bee pollen's bioavailability and functional properties, making it more suitable for use in nutraceuticals and functional foods.These treatments proved to increase the antioxidant capacity, digestibility, and create high-value ingredient for supplements, beverages, and fortified foods.

Anti-inflammatory and antioxidant activity of functional lipids extracted through sustainable technologies from Mexican Opuntia ficus-indica seeds

Opuntia ficus-indica (OFI) seeds are a rich source of functional lipids, yet research on Mexican cultivars remains limited. This study evaluated the antioxidant and anti-inflammatory properties of lipids extracted through subcritical fluid and supercritical fluid extraction with carbon dioxide (SCE-CO₂ and SFE-CO₂) from Mexican OFI Villanueva and Rojo Vigor seeds with and without enzymatic pretreatment. SCE OFI Villanueva oil showed higher extraction efficiency of linoleic (45.86 mg/g), and oleic (9.86 mg/g) acids purified more than 5.47 and 1.18 times, respectively. Additionally, SCE oils exhibited the highest antioxidant potential (68 %) and anti-inflammatory activity (45 %) at the evaluated doses. In conclusion, SCE-CO₂ enhanced the extraction efficiency of unsaturated fatty acids, improving their potential biological effects, while enzymatic pretreatment did not positively impact on results, suggesting reduced extraction efficiency and bioactivity. These findings suggest that OFI seeds can serve as a valuable source of functional ingredients for the development of value-added food products.