Recovering Valuable Chemicals from Polypropylene Waste via a Mild Catalyst-Free Hydrothermal Process.

Waste polypropylene (PP) presents a significant environmental challenge, owing to its refractory nature and inert C-C backbone. In this study, we introduce a practical chemical recovery strategy from PP waste using a mild catalyst-free hydrothermal treatment (HT). The treatment converts 64.1% of the processed PP into dissolved organic products within 2 h in an air atmosphere at 160 °C. Higher temperatures increase the PP conversion efficiency. Distinct electron absorption and emission characteristics of the products are identified by spectral analysis. Fourier transform-ion cyclotron resonance-mass spectrometry (FT-ICR-MS) reveals the oxidative cracking of PP into shorter-chain homologues (10-50 carbon atoms) containing carboxylic and carbonyl groups. Density functional theory (DFT) calculations support a reaction pathway involving thermal C-H oxidation at the tertiary carbon sites in the polymer chain. The addition of 1% H2O2 further enhances the oxidation reaction to produce valuable short-chain acetic acids, enabling gram-scale recycling of both pure PP and disposable surgical masks from the real world. Techno-economic analysis (TEA) and environmental life cycle costing (E-LCC) analysis suggest that this hydrothermal oxidation recovery technology is financially viable, which shows significant potential in tackling the ongoing plastic pollution crisis and advancing plastic treatment methodologies toward a circular economy paradigm.

Exploring the green frontier: Subcritical water chromatography for sustainable analytical practices.

Water in the subcritical state is characterized by properties significantly different from water under standard conditions. These include low viscosity, low surface tension, and a much lower dielectric constant, increasing the solubility of nonpolar substances. For this reason, it can provide an alternative solvent and be used in chromatographic techniques-subcritical water chromatography (SBWC). SBWC appears to be one of the greenest analytical techniques until we unravel chromatography with pure water at room temperature. The versatility of SBWC is explored through its applications in the separation and analysis of a wide range of compounds, including pharmaceuticals, natural products, etc. The use of subcritical water as a mobile phase requires suitable stable stationary phases and special apparatus. Still, it makes it possible to conduct analyses without using organic solvents. When using this technique, it is important to remember that it suits the analysis of thermally stable substances. The following work is a critical review of developments in SBWC.

Subcritical Water Extraction of Undaria pinnatifida: Comparative Study of the Chemical Properties and Biological Activities across Different Parts.

The subcritical water extraction of Undaria pinnatifida (blade, sporophyll, and root) was evaluated to determine its chemical properties and biological activities. The extraction was conducted at 180 °C and 3 MPa. Root extracts exhibited the highest phenolic content (43.32 ± 0.19 mg phloroglucinol/g) and flavonoid content (31.54 ± 1.63 mg quercetin/g). Sporophyll extracts had the highest total sugar, reducing sugar, and protein content, with 97.35 ± 4.23 mg glucose/g, 56.44 ± 3.10 mg glucose/g, and 84.93 ± 2.82 mg bovine serum albumin (BSA)/g, respectively. The sporophyll contained the highest fucose (41.99%) and mannose (10.37%), whereas the blade had the highest galactose (48.57%) and glucose (17.27%) content. Sporophyll had the highest sulfate content (7.76%). Key compounds included sorbitol, glycerol, L-fucose, and palmitic acid. Root extracts contained the highest antioxidant activity, with IC50 values of 1.51 mg/mL (DPPH), 3.31 mg/mL (ABTS+), and 2.23 mg/mL (FRAP). The root extract exhibited significant α-glucosidase inhibitory activity with an IC50 of 5.07 mg/mL, indicating strong antidiabetic potential. The blade extract showed notable antihypertensive activity with an IC50 of 0.62 mg/mL. Hence, subcritical water extraction to obtain bioactive compounds from U. pinnatifida, supporting their use in functional foods, cosmetics, and pharmaceuticals is highlighted. This study uniquely demonstrates the variation in bioactive compound composition and bioactivities across different parts of U. pinnatifida, providing deeper insights. Significant correlations between chemical properties and biological activities emphasize the use of U. pinnatifida extracts for chronic conditions.

Simultaneous synthesis of super-paramagnetic hydrochar in a one-pot using subcritical water medium and evaluation of its photocatalytic activity.

The unregulated release of chemical dyes into the environment presents considerable environmental hazards when left untreated. Photocatalytic degradation, acknowledged as an eco-friendly and cost-effective method, has garnered attention for its efficacy in eliminating organic pollutants like dye. Consequently, the development of multifunctional materials with different applications in environmental and catalytic fields emerges as a promising avenue. Recognizing the significance of integrating catalysts and porous materials for enhancing interactions between pollutants and photo-sensitive substances, magnetic hydrochar emerges as a solution offering heightened efficiency, scalability, recyclability, and broad applicability in various environmental processes, notably wastewater treatment, due to its facile separation capability. In this study, Fe3O4-based, super-paramagnetic hydrochar (SMHC) was simultaneously synthesized in a single step using a coconut shell in the subcritical water medium. A thorough analysis was conducted on both raw hydrochar (RHC) and SMHC to unravel the mechanism of interaction between Fe3O4 nanoparticles and the hydrochar matrix. The synthesized hydrochar exhibited super-paramagnetic characteristics, with a saturation magnetization of 23.7 emu/g and a magnetic hysteresis loop. SMHC displayed a BET surface area of 42.6 m2/g and an average pore size of 26.3 nm, indicating a mesoporous structure according to nitrogen adsorption-desorption isotherms. XRD analysis revealed magnetic crystal sizes in the obtained SMHC to be 13.7 nm. The photocatalytic performance of SMHC was evaluated under visible light exposure in the presence of H2O2 for Astrazon yellow (AY) dye degradation, with optimization conducted using response surface methodology (RSM). The most substantial dye removal, reaching 92.83%, was achieved with 0.4% H2O2 at a 20 mg/L dye concentration and an 80-min reaction duration.

Obtaining Cellulose Fibers from Almond Shell by Combining Subcritical Water Extraction and Bleaching with Hydrogen Peroxide.

Almond shell (AS) represents about 33% of the almond fruit, being a cellulose-rich by-product. The use of greener methods for separating cellulose would contribute to better exploitation of this biomass. Subcritical water extraction (SWE) at 160 and 180 °C has been used as a previous treatment to purify cellulose of AS, followed by a bleaching step with hydrogen peroxide (8%) at pH 12. For comparison purposes, bleaching with sodium chlorite of the extraction residues was also studied. The highest extraction temperature promoted the removal of hemicellulose and the subsequent delignification during the bleaching step. After bleaching with hydrogen peroxide, the AS particles had a cellulose content of 71 and 78%, with crystallinity index of 50 and 62%, respectively, for those treated at 160 and 180 °C. The use of sodium chlorite as bleaching agent improved the cellulose purification and crystallinity index. Nevertheless, cellulose obtained by both bleaching treatments could be useful for different applications. Therefore, SWE represents a promising green technique to improve the bleaching sensitivity of lignocellulosic residues, such as AS, allowing for a great reduction in chemicals in the cellulose purification processes.

A Review: Subcritical Water Extraction of Organic Pollutants from Environmental Matrices.

Most organic pollutants are serious environmental concerns globally due to their resistance to biological, chemical, and photolytic degradation. The vast array of uses of organic compounds in daily life causes a massive annual release of these substances into the air, water, and soil. Typical examples of these substances include pesticides, polychlorinated biphenyls (PCBs), and polycyclic aromatic hydrocarbons (PAHs). Since they are persistent and hazardous in the environment, as well as bio-accumulative, sensitive and efficient extraction and detection techniques are required to estimate the level of pollution and assess the ecological consequences. A wide variety of extraction methods, including pressurized liquid extraction, microwave-assisted extraction, supercritical fluid extraction, and subcritical water extraction, have been recently used for the extraction of organic pollutants from the environment. However, subcritical water has proven to be the most effective approach for the extraction of a wide range of organic pollutants from the environment. In this review article, we provide a brief overview of the subcritical water extraction technique and its application to the extraction of PAHs, PCBs, pesticides, pharmaceuticals, and others form environmental matrices. Furthermore, we briefly discuss the influence of key extraction parameters, such as extraction time, pressure, and temperature, on extraction efficiency and recovery.

A broad assessment of Eremurus spectabilis M. Bieb: chemical and elemental composition, total phenolic and antimicrobial activity analysis, and quantum chemical calculations of radical scavenging potential.

Eremurus spectabilis M. Bieb was extensively investigated experimentally and theoretically, including the antioxidant properties of compounds such as flavonoids, hydroxycinnamic acid derivatives, hydroxybenzoic acid derivatives, and organic acids. Antioxidant activity was investigated using the Density Functional Theory (DFT) method based on three known mechanisms: hydrogen atom transfer (HAT), single electron transfer followed by proton transfer (SET-PT), and sequential proton loss electron transfer (SPLET). Subcritical water extraction (SWE), soxhlet extraction (SE), and solvent extraction (SOE) techniques were applied in the extraction process. Malic acid was the major compound with an extract concentration of 38,532.84 ± 1849.58 µg analyte/kg, total phenolics, and free radical scavenging activity were 10.67 mg gallic acid/mL extract and 73.89% per mg/mL extract, respectively. P, Fe, Na, Mg, K, and Ca were the main elements. The antibacterial activity of E. spectabilis against seven bacteria was evaluated, and it was found to be higher than the commercial antibiotics P10 and AMC30.

Unlocking the potential of Allium dictyoprasum C.A. Meyer ex Kunth: quantum chemical insights into radical scavenging, chemical composition, phenolic content, and antimicrobial activity.

Allium dictyoprasum C.A. Meyer ex Kunth (A. dictyoprasum) underwent comprehensive analysis, encompassing quantum chemical computations to assess its radical scavenging potential, chemical and elemental composition, total phenolic content, and antimicrobial activity. Experimental and theoretical investigations focused on elucidating the radical scavenging properties of polyhydroxy phenolic compounds present in the plant. Quantum chemical calculations were employed to evaluate the antioxidants employed to evaluate selected polyhydroxy phenolic molecules including flavonoids, hydrocinnamic acid derivatives, and hydroxybenzoic acid derivatives from natural sources. Thermochemical parameters of these compounds were calculated by the B3LYP/6-311 G++(d,p) level in both gas and solvent phases to elucidate the radical scavenging mechanism including hydrogen atom transfer (HAT), single electron transfer followed by proton transfer (SET-PT) and sequential proton loss electron transfer (SPLET). Analysis of A. dictyoprasum extracts obtained via various extraction methods revealed the presence of several major compounds, including dimethyl trisulfide, 3,5-Dihydroxy-6-methyl-2,3-dihydro-4 H-pyran-4-one, 2-Methoxy-4-vinylphenol, Dimethyl phthalate, Methyl palmitate, Methyl oleate, Methyl stearate, (9Z)-9-Octadecenamide. Notably, Malic acid and Quinic acid were identified as major compounds, with concentrations of 43.31 and 17.47 mg kg-1 extract, respectively, based on LC-MS/MS analysis. The total phenolic content of the extract was measured as 17.83 mg gallic acid/mL, while its free radical scavenging activity was 80.89% per mg/mL. Elemental analysis revealed significant levels of Mg, K, Na, Fe, and P, with minor concentrations of elements such as Ti, Tl, B, and Be. Furthermore, A. dictyoprasum exhibited notable antibacterial activity against various bacteria strains, surpassing the efficacy of some commercial antibiotics.

Quantum chemical calculations of radical scavenging analysis were performed.Thermochemical parameters were calculated by the B3LYP/6­311 G++(d,p) level.Radical scavenging mechanism was evaluated based on HAT, SET-PT and SPLET.Chemical composition of Allium dictyoprasum C.A. Meyer ex Kunth was determined.A. dictyoprasum has a greater antibacterial effects than some commercial antibiotics.

Subcritical water extraction of Equisetum arvense biomass withdraws cell wall fractions that trigger plant immune responses and disease resistance.

Plant cell walls are complex structures mainly made up of carbohydrate and phenolic polymers. In addition to their structural roles, cell walls function as external barriers against pathogens and are also reservoirs of glycan structures that can be perceived by plant receptors, activating Pattern-Triggered Immunity (PTI). Since these PTI-active glycans are usually released upon plant cell wall degradation, they are classified as Damage Associated Molecular Patterns (DAMPs). Identification of DAMPs imply their extraction from plant cell walls by using multistep methodologies and hazardous chemicals. Subcritical water extraction (SWE) has been shown to be an environmentally sustainable alternative and a simplified methodology for the generation of glycan-enriched fractions from different cell wall sources, since it only involves the use of water. Starting from Equisetum arvense cell walls, we have explored two different SWE sequential extractions (isothermal at 160 ºC and using a ramp of temperature from 100 to 160 ºC) to obtain glycans-enriched fractions, and we have compared them with those generated with a standard chemical-based wall extraction. We obtained SWE fractions enriched in pectins that triggered PTI hallmarks in Arabidopsis thaliana such as calcium influxes, reactive oxygen species production, phosphorylation of mitogen activated protein kinases and overexpression of immune-related genes. Notably, application of selected SWE fractions to pepper plants enhanced their disease resistance against the fungal pathogen Sclerotinia sclerotiorum. These data support the potential of SWE technology in extracting PTI-active fractions from plant cell wall biomass containing DAMPs and the use of SWE fractions in sustainable crop production.

Field testing of transgenic aspen from large greenhouse screening identifies unexpected winners.

Trees constitute promising renewable feedstocks for biorefinery using biochemical conversion, but their recalcitrance restricts their attractiveness for the industry. To obtain trees with reduced recalcitrance, large-scale genetic engineering experiments were performed in hybrid aspen blindly targeting genes expressed during wood formation and 32 lines representing seven constructs were selected for characterization in the field. Here we report phenotypes of five-year old trees considering 49 traits related to growth and wood properties. The best performing construct considering growth and glucose yield in saccharification with acid pretreatment had suppressed expression of the gene encoding an uncharacterized 2-oxoglutarate-dependent dioxygenase (2OGD). It showed minor changes in wood chemistry but increased nanoporosity and glucose conversion. Suppressed levels of SUCROSE SYNTHASE, (SuSy), CINNAMATE 4-HYDROXYLASE (C4H) and increased levels of GTPase activating protein for ADP-ribosylation factor ZAC led to significant growth reductions and anatomical abnormalities. However, C4H and SuSy constructs greatly improved glucose yields in saccharification without and with pretreatment, respectively. Traits associated with high glucose yields were different for saccharification with and without pretreatment. While carbohydrates, phenolics and tension wood contents positively impacted the yields without pretreatment and growth, lignin content and S/G ratio were negative factors, the yields with pretreatment positively correlated with S lignin and negatively with carbohydrate contents. The genotypes with high glucose yields had increased nanoporosity and mGlcA/Xyl ratio, and some had shorter polymers extractable with subcritical water compared to wild-type. The pilot-scale industrial-like pretreatment of best-performing 2OGD construct confirmed its superior sugar yields, supporting our strategy.

Exploring Bioactive Compounds in Brown Seaweeds Using Subcritical Water: A Comprehensive Analysis.

In this study, we characterized the bioactive properties of three important brown seaweed species, Sargassum thunbergii, Undaria pinnatifida, and Saccharina japonica, by subcritical water extraction (SWE), as these species are well known for their beneficial health effects. Their physiochemical properties, including potential antioxidant, antihypertensive, and α-glucosidase inhibitory activity, and the antibacterial activity of the hydroysates were also analyzed. The highest total phlorotannin, total sugar content, and reducing sugar content in the S. thunbergii hydrolysates were 38.82 ± 0.17 mg PGE/g, 116.66 ± 0.19 mg glucose/g dry sample, and 53.27 ± 1.57 mg glucose/g dry sample, respectively. The highest ABTS+ and DPPH antioxidant activities were obtained in the S. japonica hydrolysates (124.77 ± 2.47 and 46.35 ± 0.01 mg Trolox equivalent/g, respectively) and the highest FRAP activity was obtained in the S. thunbergii hydrolysates (34.47 ± 0.49 mg Trolox equivalent/g seaweed). In addition, the seaweed extracts showed antihypertensive (≤59.77 ± 0.14%) and α-glucosidase inhibitory activity (≤68.05 ± 1.15%), as well as activity against foodborne pathogens. The present findings provide evidence of the biological activity of brown seaweed extracts for potential application in the food, pharmaceutical, and cosmetic sectors.

In Vitro Biodegradation, Drug Absorption, and Physical Properties of Gelatin-Fucoidan Microspheres Made of Subcritical-Water-Modified Fish Gelatin.

This study aimed to prepare gelatin-fucoidan microspheres with enhanced doxorubicin binding efficiency and controllable biodegradation using fish gelatin combined with low molecular weight (LMW) gelatin and fucoidan at fixed ratios. The MW of gelatin was modified by subcritical water (SW), which is known as a safe solvent, at 120 °C, 140 °C, and 160 °C. In addition, gelatin-fucoidan microspheres were prepared using a solvent exchange technique. Our findings revealed that particle size decreased, the surface was rougher, the swelling ratio increased, and particle shape was irregular in microspheres composed of SW-modified gelatin. Doxorubicin binding efficiency was improved by fucoidan and SW-modified gelatin at 120 °C but not at 140 °C and 160 °C. Interestingly, an increase in in vitro enzymatic degradation was observed in the microspheres consisting of SW-modified fish gelatin, although the cross-linking degree between them was not significantly different. This is because LMW gelatin could form more cross-linked bonds, which might be weaker than the intramolecular bonds of gelatin molecules. Gelatin-fucoidan microspheres consisting of SW-modified fish gelatin with controlled biodegradation rates could be a candidate for a short-term transient embolization agent. In addition, SW would be a promising method to modify the MW of gelatin for medical applications.

Optimizing the Production of Antioxidant and Antibacterial Alkaloids from Macleaya cordata by Subcritical Water Extraction Technology.

In this work, the subcritical water extraction technology was used to extract alkaloids from Macleaya cordata, and the effects of extraction temperature and time on its yield were investigated to find the best extraction conditions. Moreover, the antioxidant capacity and antibacterial activity of Macleaya cordata extract were studied. Furthermore, through the single-factor method, it was found that properly increasing the extraction temperature and prolonging the extraction time was conducive to increasing alkaloid yield. Still, a considerable amount of alkaloids might be decomposed by heat, resulting in a decrease in their yield. The results showed that the optimal extraction temperature of alkaloids from Macleaya cordata with subcritical water is 190 °C, the time is 45 min, and the corresponding maximum yield is 35.19±0.12 mg/g (sanguinarine equivalent in raw materials). In addition, the antioxidation and bacteriostasis abilities of subcritical water extract are better than those of traditional hot water extract, indicating that it is a feasible method to extract alkaloids from Macleaya cordata with subcritical water.

Subcritical Water Extraction of Phenolic Compounds from Vaccinium Dunalianum Wight Leaves and Their Antioxidant and Tyrosinase Inhibitory Activities in Vitro.

Subcritical water extraction was used to extract bioactive phenolic compounds from Vaccinium dunalianum Wight leaves. The optimal extraction conditions were determined as an extraction temperature of 150 °C, an extraction time of 40 min, and a liquid-solid ratio of 35 : 1 mL/g. The total phenolic content reached 21.35 mg gallic acid /g, which was 16 % higher than that by hot water extraction. The subcritical water extraction extract exhibited strong scavenging activity of DPPH free radical and ABTS+ free radical, as well as significant tyrosinase inhibitory activity. The study suggests that subcritical water extraction can alter the composition of the extracts, leading to the production of various phenolic compounds, effective antioxidants, and tyrosinase inhibitors from Vaccinium dulciana Wight leaves. These findings confirm the potential of Vaccinium dunalianum Wight as a natural antioxidant molecule source for the medicine and food industries, and for the therapy of skin pigmentation disorders.

Solubility and Decomposition of Organic Compounds in Subcritical Water.

In this article, studies on organic solubility and stability in subcritical water reported during the past 25 years have been reviewed. Data on the solubility and decomposition of organic compounds in subcritical water, a green solvent, are needed in environmental remediation, chemistry, chemical engineering, medicine, polymer, food, agriculture, and many other fields. For solubility studies, the experimental systems used to measure solubility, mathematical equations derived and applied for the modeling of the experimentally determined solubility data, and the correlation between the predicated and experimental data have been summarized and discussed. This paper also reviewed organic decomposition under subcritical water conditions. In general, the solubility of organics is significantly enhanced with increasing water temperature. Likewise, the percentage of organic decomposition also increases with higher temperature.

Efficient Mineralization of Fluoroelastomers Using Superheated Water in the Presence of Potassium Hydroxide.

The mineralization of fluoroelastomers (FKMs) in superheated water in the presence of potassium hydroxide (KOH) was investigated with the aim of developing a methodology for recycling the fluorine element. Two FKMs-an "uncrosslinked FKM", representing a poly(vinylidene fluoride-co-hexafluoropropylene) (poly(VDF-co-HFP)) copolymer with a VDF/HFP molar ratio of 78/22 and a "crosslinked FKM" consisting of this copolymer (cured by peroxide) and carbon black-were treated. The fluorine content of these FKMs was efficiently transformed into F- ions in the reaction solution using low KOH concentrations (0.10-0.50 M) at 200-250 °C. When the uncrosslinked or crosslinked FKMs reacted with aqueous KOH (0.20 M) at a rather low temperature (200 °C) for 18 h, the fluorine content of these FKMs was completely mineralized (both F- yields were 100%). Although the crosslinked FKM contained carbon black, the fluorine mineralization of the FKM was not inhibited. The addition of Ca(OH)2 to the reaction solutions after the superheated water treatment at 250 °C for 6 h with aqueous KOH (0.50 M) led to the production of pure CaF2, identified using X-ray spectroscopy, with 100% and 93% yields for the uncrosslinked and crosslinked FKMs, respectively.

Degradation and Extraction of Organochlorine Pollutants from Environmental Solids under Subcritical Water Conditions.

A subcritical water degradation and extraction method was developed to remediate environmental soils contaminated by highly recalcitrant organochlorine pollutants. Hydrogen peroxide was used to effectively decompose organochlorine pollutants under subcritical water conditions. As a method optimization study, the static wet oxidation of chlorophenols was first performed in subcritical water with and without added hydrogen peroxide. Complete oxidation was achieved using an added oxidant, and thus, the oxidation and extraction of chlorophenols from a sand matrix was then attempted. Complete oxidation and extraction with added oxidant were achieved within 30 min at 100 °C. We then investigated the subcritical water degradation and extraction of dieldrin, mirex, and p,p'-DDD. These organochlorine pesticides were not as easily oxidized as the chlorophenols, and the benefit of adding hydrogen peroxide was only clearly observed at 200 °C. Approximately a 20% increase in degradation was noted for each pesticide and insecticide at this temperature. Unfortunately, this difference was not observed with an increase in temperature to 250 °C, except in some cases, where the amount of degradation byproducts was reduced. Dieldrin and p,p'-DDD were essentially destroyed at 250 °C, while all the pesticides and the insecticides were completely removed from the sand at this temperature. The proposed method was then used to remediate a soil sample highly contaminated with DDT. The soil was obtained from the grounds of an old DDT mixing facility in Virginia and has been aging for several decades. Not only was 100% removal of DDT from this soil achieved using the proposed method at 250 °C, but also, the extracted DDT was completely destroyed during the process. The proposed remediation method, therefore, demonstrates a high potential as an efficient and environmentally sound technique for the detoxification of soils.

Subcritical Water Extraction of Onosma mutabilis: Process Optimization and Chemical Profile of the Extracts.

The aboveground and root parts of Onosma mutabilis were extracted using subcritical water and the process was optimized with response surface methodology. The composition of the extracts was determined by chromatographic methods and compared to that of conventional maceration of the plant. The optimum total phenolic contents for the aboveground part and the roots were 193.9 and 174.4 µg/g, respectively. These results were achieved at a subcritical water temperature of 150 °C, an extraction time of 180 min, and a water/plant ratio of 0.1, for both parts of the plant. Principal component analysis revealed that the roots contained mainly phenols, ketones, and diols, with the aboveground part mostly alkenes and pyrazines, whereas the extract from maceration contained mainly terpenes, esters, furans, and organic acids. The quantification of selected phenolic substances showed that subcritical water extraction compared favorably to maceration, especially with respect to pyrocatechol (1062 as compared to 10.2 µg/g) and epicatechin (1109 as compared to 23.4 µg/g). Furthermore, the roots of the plant contained twice as much of these two phenolics compared to the aboveground part. Subcritical water extraction of O. mutabilis is an environmentally friendly method that can extract selected phenolics at higher concentrations compared to maceration.

Application of Green Technology to Extract Clean and Safe Bioactive Compounds from Tetradesmus obliquus Biomass Grown in Poultry Wastewater.

Microalgae are capable of assimilating nutrients from wastewater (WW), producing clean water and biomass rich in bioactive compounds that need to be recovered from inside the microalgal cell. This work investigated subcritical water (SW) extraction to collect high-value compounds from the microalga Tetradesmus obliquus after treating poultry WW. The treatment efficiency was evaluated in terms of total Kjeldahl nitrogen (TKN), phosphate, chemical oxygen demand (COD) and metals. T. obliquus was able to remove 77% TKN, 50% phosphate, 84% COD, and metals (48-89%) within legislation values. SW extraction was performed at 170 °C and 30 bar for 10 min. SW allowed the extraction of total phenols (1.073 mg GAE/mL extract) and total flavonoids (0.111 mg CAT/mL extract) with high antioxidant activity (IC50 value, 7.18 µg/mL). The microalga was shown to be a source of organic compounds of commercial value (e.g., squalene). Finally, the SW conditions allowed the removal of pathogens and metals in the extracts and residues to values in accordance with legislation, assuring their safety for feed or agriculture applications.

Isolation of Garlic Bioactives by Pressurized Liquid and Subcritical Water Extraction.

Garlic (Allium sativum L.) is widely used in various food products and traditional medicine. Besides unique taste and flavour, it is well known for its chemical profile and bioactive potential. The aim of this study was to apply subcritical water extraction (SWE) and pressurized liquid extraction (PLE) for the extraction of bioactive compounds from the Ranco genotype of garlic. Moreover, PLE process was optimized using response surface methodology (RSM) in order to determine effects and optimize ethanol concentration (45-75%), number of cycles (1-3), extraction time (1-3 min) and temperature (70-110 °C) for maximized total phenols content (TP) and antioxidant activity evaluated by various in vitro assays. Furthermore, temperature effect in SWE process on all responses was evaluated, while allicin content (AC), as a major organosulphur compound, was determined in all samples. Results indicated that PLE provided tremendous advantage over SWE in terms of improved yield and antioxidant activity of garlic extracts. Therefore, high-pressure processes could be used as clean and green procedures for the isolation of garlic bioactives.