This study aimed to enhance the dissolution rate of Teriflunomide, a medication for multiple sclerosis that exhibits low water solubility despite its high permeability. To tackle this issue, the Gas Antisolvent technique was utilized to decrease the particle size of Teriflunomide. Three critical parameters were examined: pressure (10, 13, and 16 MPa), temperature (308, 318, and 328 K), and the ratio of Teriflunomide to Hydroxypropyl methylcellulose (1, 5, and 9 w/w). The optimization of these variables was carried out using the Box-Behnken Design method. The coprecipitation of Teriflunomide with Hydroxypropyl methylcellulose was investigated under optimal conditions (16 MPa, 315 K, and a 1 w/w ratio). DSC, XRD, FTIR, SEM, and DLS were employed to examine and characterize the thermal stability, crystallinity, and to assess the shape and position of the absorption peaks, as well as the morphology and particle size. The resulting TEF-HPMC nanoparticles were measured at 561 ± 25 nm, which was found to be significantly smaller than the original sample (125 ± 28 μm).
{"title":"Production of teriflunomide-hydroxypropyl methyl cellulose composites utilizing the Gas Antisolvent (GAS) process and Box-Behnken Design","authors":"Mahshid Askarizadeh , Nadia Esfandiari , Bizhan Honarvar , Seyed Ali Sajadian , Amin Azdarpour","doi":"10.1016/j.supflu.2025.106820","DOIUrl":"10.1016/j.supflu.2025.106820","url":null,"abstract":"<div><div>This study aimed to enhance the dissolution rate of Teriflunomide, a medication for multiple sclerosis that exhibits low water solubility despite its high permeability. To tackle this issue, the Gas Antisolvent technique was utilized to decrease the particle size of Teriflunomide. Three critical parameters were examined: pressure (10, 13, and 16 MPa), temperature (308, 318, and 328 K), and the ratio of Teriflunomide to Hydroxypropyl methylcellulose (1, 5, and 9 w/w). The optimization of these variables was carried out using the Box-Behnken Design method. The coprecipitation of Teriflunomide with Hydroxypropyl methylcellulose was investigated under optimal conditions (16 MPa, 315 K, and a 1 w/w ratio). DSC, XRD, FTIR, SEM, and DLS were employed to examine and characterize the thermal stability, crystallinity, and to assess the shape and position of the absorption peaks, as well as the morphology and particle size. The resulting TEF-HPMC nanoparticles were measured at 561 ± 25 nm, which was found to be significantly smaller than the original sample (125 ± 28 μm).</div></div>","PeriodicalId":17078,"journal":{"name":"Journal of Supercritical Fluids","volume":"229 ","pages":"Article 106820"},"PeriodicalIF":4.4,"publicationDate":"2025-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145323371","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-10-15DOI: 10.1016/j.supflu.2025.106819
Kelly Roberta Pinheiro Pantoja , Giselle Cristine Melo Aires , Sophia Aimy Oppata , João Pedro Ferraz de Carvalho , Renato Macedo Cordeiro , Raul Nunes de Carvalho Junior
This study investigates the extraction of avocado oil from the Margarida variety using supercritical CO₂, with the aim of obtaining a product of superior quality compared to commercial avocado oil from the Hass variety, obtained by cold pressing. The quality of the oils was evaluated in terms of their physicochemical properties, composition of bioactive compounds (fatty acids, lutein, phenolic compounds, and α-tocopherol), and nutritional quality indices. Additionally, the study assessed the reproducibility of Ultra-Performance Convergence Chromatography (UPC²) compared to Gas Chromatography coupled with Mass Spectrometry (GC/MS) for the analysis of fatty acid profiles. The supercritical extraction yielded a high yield (44.90 %) and produced an oil with low levels of free fatty acids (1.04 %) and peroxides (7.03 meq/kg). The oil is rich in natural antioxidants, such as lutein (113.32 µg/g), phenolic compounds (137.75 µg GAE/g), and α-tocopherol (51.90 µg/g), and has a high concentration of beneficial fatty acids, with 44.41 % oleic acid and 28.37 % linoleic acid. With an excellent nutritional profile, evidenced by low atherogenic and thrombogenic indices. Statistical tests indicated no significant differences between the chromatographic techniques. Margarida oil demonstrates nutritional and functional properties superior to commercial Hass oil.
{"title":"High-quality margarida avocado oil obtained by Sc-CO2 compared to commercial hass avocado oil from cold pressing and comparative lipid profile analysis by UPC² and GC/MS","authors":"Kelly Roberta Pinheiro Pantoja , Giselle Cristine Melo Aires , Sophia Aimy Oppata , João Pedro Ferraz de Carvalho , Renato Macedo Cordeiro , Raul Nunes de Carvalho Junior","doi":"10.1016/j.supflu.2025.106819","DOIUrl":"10.1016/j.supflu.2025.106819","url":null,"abstract":"<div><div>This study investigates the extraction of avocado oil from the Margarida variety using supercritical CO₂, with the aim of obtaining a product of superior quality compared to commercial avocado oil from the Hass variety, obtained by cold pressing. The quality of the oils was evaluated in terms of their physicochemical properties, composition of bioactive compounds (fatty acids, lutein, phenolic compounds, and α-tocopherol), and nutritional quality indices. Additionally, the study assessed the reproducibility of Ultra-Performance Convergence Chromatography (UPC²) compared to Gas Chromatography coupled with Mass Spectrometry (GC/MS) for the analysis of fatty acid profiles. The supercritical extraction yielded a high yield (44.90 %) and produced an oil with low levels of free fatty acids (1.04 %) and peroxides (7.03 meq/kg). The oil is rich in natural antioxidants, such as lutein (113.32 µg/g), phenolic compounds (137.75 µg GAE/g), and α-tocopherol (51.90 µg/g), and has a high concentration of beneficial fatty acids, with 44.41 % oleic acid and 28.37 % linoleic acid. With an excellent nutritional profile, evidenced by low atherogenic and thrombogenic indices. Statistical tests indicated no significant differences between the chromatographic techniques. Margarida oil demonstrates nutritional and functional properties superior to commercial Hass oil.</div></div>","PeriodicalId":17078,"journal":{"name":"Journal of Supercritical Fluids","volume":"229 ","pages":"Article 106819"},"PeriodicalIF":4.4,"publicationDate":"2025-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145364354","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The integrated preparation strategy of multi-layer foam materials is expected to meet the demand for frequency-selective electromagnetic shielding properties. In this study, a synergistic regulation strategy of magnetic field and supercritical CO2 foaming technology was employed to achieve the parallel alternate arrangement of conductive layers and porous layers. The impact of the layered cell structure in liquid silicone rubber/ ferrosoferric oxide modified graphene/ carbon nanotube (LSR/Fe3O4@G/CNT) on the electromagnetic shielding performance in the X-band (8.4 GHz–12.4 GHz) was systematically investigated. The results demonstrate that the electromagnetic shielding effectiveness (SET) of the unfoamed material remained stable at 11.4 dB. In contrast, the layered foam material exhibited frequency-selective electromagnetic shielding characteristics and the maximum SET reaching 33.4 dB after foaming. By adjusting the foaming parameters, the position of the shielding peak can be effectively regulated, enabling the multi-layered silicone rubber foam to achieve high shielding efficiency within specific frequency bands.
{"title":"Multilayer integrated design for frequency-tunable silicone rubber-based electromagnetic shielding foams","authors":"Zuoze Fan, Xiaohan Wang, Bo Wang, Yishen Zhao, Ruyun Xu, Guangxian Li, Xia Liao","doi":"10.1016/j.supflu.2025.106818","DOIUrl":"10.1016/j.supflu.2025.106818","url":null,"abstract":"<div><div>The integrated preparation strategy of multi-layer foam materials is expected to meet the demand for frequency-selective electromagnetic shielding properties. In this study, a synergistic regulation strategy of magnetic field and supercritical CO<sub>2</sub> foaming technology was employed to achieve the parallel alternate arrangement of conductive layers and porous layers. The impact of the layered cell structure in liquid silicone rubber/ ferrosoferric oxide modified graphene/ carbon nanotube (LSR/Fe<sub>3</sub>O<sub>4</sub>@G/CNT) on the electromagnetic shielding performance in the X-band (8.4 GHz–12.4 GHz) was systematically investigated. The results demonstrate that the electromagnetic shielding effectiveness (<em>SE</em><sub>T</sub>) of the unfoamed material remained stable at 11.4 dB. In contrast, the layered foam material exhibited frequency-selective electromagnetic shielding characteristics and the maximum <em>SE</em><sub>T</sub> reaching 33.4 dB after foaming. By adjusting the foaming parameters, the position of the shielding peak can be effectively regulated, enabling the multi-layered silicone rubber foam to achieve high shielding efficiency within specific frequency bands.</div></div>","PeriodicalId":17078,"journal":{"name":"Journal of Supercritical Fluids","volume":"229 ","pages":"Article 106818"},"PeriodicalIF":4.4,"publicationDate":"2025-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145364355","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-10-11DOI: 10.1016/j.supflu.2025.106814
A. Pizzano , S.B. Rodriguez Reartes , P.E. Hegel
In the last years, there has been an increasing use of eco-friendly lubricant options produced from renewable raw materials, which are less toxic to humans and ecosystems. As the demand for sustainable products rises, lubricants derived from vegetable oils and animal fats are gaining attraction. In this study, we evaluate the purification of a biolubricant synthesized via classical alkali-catalyst esterification of fatty acid methyl esters (FAME) with trimethylolpropane (TMP) using CO2 as solvent media. Unlike conventional purification solvents, using CO2 minimizes environmental impact and aligns with green chemistry principles. We investigate the purification and upgrading of the filtrated biolubricant (28 wt% FAME) using CO2 -both in its liquid and supercritical states- as a green solvent for designing a more sustainable separation process. The study examines phase equilibria of the multicomponent mixture (liquid-liquid-vapor to liquid-vapor phase transition), solubility of biolubricant in CO2 (8.0–22.4 mg/g biolubricant/CO2 according to operating conditions) and the purification process. The final bio-based base oils are analyzed to determine their FAME content, viscosity, and viscosity index. Results show that purified bio-based base oils contain as little as 2.9 wt% FAME, with a viscosity of 0.051 Pa.s at 313.2 K and a viscosity index of 196, comparable to those of the trimethylolpropane triolein standard. These findings suggest that the bio-based base oils produced and purified are suitable for lubrication applications, matching or exceeding the quality of conventional lubricants.
{"title":"Upgrading and purification of biolubricants by extraction of fatty acid methyl esters with dense CO2","authors":"A. Pizzano , S.B. Rodriguez Reartes , P.E. Hegel","doi":"10.1016/j.supflu.2025.106814","DOIUrl":"10.1016/j.supflu.2025.106814","url":null,"abstract":"<div><div>In the last years, there has been an increasing use of eco-friendly lubricant options produced from renewable raw materials, which are less toxic to humans and ecosystems. As the demand for sustainable products rises, lubricants derived from vegetable oils and animal fats are gaining attraction. In this study, we evaluate the purification of a biolubricant synthesized via classical alkali-catalyst esterification of fatty acid methyl esters (FAME) with trimethylolpropane (TMP) using CO<sub>2</sub> as solvent media. Unlike conventional purification solvents, using CO<sub>2</sub> minimizes environmental impact and aligns with green chemistry principles. We investigate the purification and upgrading of the filtrated biolubricant (28 wt% FAME) using CO<sub>2</sub> -both in its liquid and supercritical states- as a green solvent for designing a more sustainable separation process. The study examines phase equilibria of the multicomponent mixture (liquid-liquid-vapor to liquid-vapor phase transition), solubility of biolubricant in CO<sub>2</sub> (8.0–22.4 mg/g biolubricant/CO<sub>2</sub> according to operating conditions) and the purification process. The final bio-based base oils are analyzed to determine their FAME content, viscosity, and viscosity index. Results show that purified bio-based base oils contain as little as 2.9 wt% FAME, with a viscosity of 0.051 Pa.s at 313.2 K and a viscosity index of 196, comparable to those of the trimethylolpropane triolein standard. These findings suggest that the bio-based base oils produced and purified are suitable for lubrication applications, matching or exceeding the quality of conventional lubricants.</div></div>","PeriodicalId":17078,"journal":{"name":"Journal of Supercritical Fluids","volume":"229 ","pages":"Article 106814"},"PeriodicalIF":4.4,"publicationDate":"2025-10-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145322498","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-10-11DOI: 10.1016/j.supflu.2025.106804
Jiawei Zhao , Lifeng Yang , Feiyu Chen , Wendeng Jiang , Mian Hu , Zhongting Hu , Zhiyan Pan , Junliang Wang
316 L stainless steel (316 L SS) is an important candidate material for super/subcritical water oxidation facilities; however, corrosion negatively affects its service life, especially in the presence of halogen ions such as chlorine. In this work, Ti-6Al-4V (TC4) coatings were deposited on 316 L SS substrates by cold spraying (CS) and subsequently remelted by laser remelting (LR). The corrosion resistance of the coatings was evaluated in subcritical (260 °C, 15.7 MPa) and supercritical (380 °C, 22.3 MPa) water containing 3.5 wt% NaCl and 3.0 wt% H2O2 for up to 300 h. Scanning electron microscopy/energy-dispersive X-ray spectroscopy (SEM/EDS) analysis revealed that LR effectively densified the coating surface and enhanced its structural integrity. Corrosion assessments based on weight change, SEM, EDS, and X-ray computed tomography (CT) indicated that the TC4 coating significantly improved the corrosion resistance of 316 L SS by inhibiting the outward diffusion of metallic elements and the inward diffusion of oxygen. X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) analyses showed that the oxide film formed on the TC4 coating consisted mainly of Ti, Al, Fe, and Cr oxides, and the inhibition effect of the coating on the matrix elements varied after different treatment processes. In particular, the 0.6 mm laser-enhanced coating has a lower corrosion weight change, a more uniform and dense corrosion surface, and a better inhibition. The combination of CS and LR is demonstrated to be an effective approach for enhancing the corrosion resistance of 316 L SS, showing great potential for application in super/subcritical water oxidation reactors.
316 L不锈钢(316 L SS)是超/亚临界水氧化设施的重要候选材料;然而,腐蚀会对其使用寿命产生负面影响,特别是在氯等卤素离子存在的情况下。采用冷喷涂(CS)技术在316 L SS基板上沉积Ti-6Al-4V (TC4)涂层,然后采用激光重熔(LR)技术进行重熔。在含3.5 wt% NaCl和3.0 wt% H2O2的亚临界水(260°C, 15.7 MPa)和超临界水(380°C, 22.3 MPa)中对涂层的耐蚀性进行了测试,测试时间为300 h。扫描电镜/能谱分析(SEM/EDS)表明,LR有效致密化了涂层表面,增强了涂层的结构完整性。基于重量变化、SEM、EDS和x射线计算机断层扫描(CT)的腐蚀评估表明,TC4涂层通过抑制金属元素的向外扩散和氧的向内扩散,显著提高了316 L SS的耐蚀性。x射线衍射(XRD)和x射线光电子能谱(XPS)分析表明,TC4涂层上形成的氧化膜主要由Ti、Al、Fe和Cr氧化物组成,不同处理工艺对基体元素的抑制效果不同。特别是0.6 mm激光增强涂层的腐蚀重量变化更小,腐蚀表面更均匀致密,缓蚀性更好。CS和LR的结合是提高316 L SS耐腐蚀性能的有效途径,在超/亚临界水氧化反应器中具有很大的应用潜力。
{"title":"Microstructure and corrosion of cold-sprayed/laser-remelted TC4 coatings on 316 L SS in oxygenated NaCl-containing super/subcritical water","authors":"Jiawei Zhao , Lifeng Yang , Feiyu Chen , Wendeng Jiang , Mian Hu , Zhongting Hu , Zhiyan Pan , Junliang Wang","doi":"10.1016/j.supflu.2025.106804","DOIUrl":"10.1016/j.supflu.2025.106804","url":null,"abstract":"<div><div>316 L stainless steel (316 L SS) is an important candidate material for super/subcritical water oxidation facilities; however, corrosion negatively affects its service life, especially in the presence of halogen ions such as chlorine. In this work, Ti-6Al-4V (TC4) coatings were deposited on 316 L SS substrates by cold spraying (CS) and subsequently remelted by laser remelting (LR). The corrosion resistance of the coatings was evaluated in subcritical (260 °C, 15.7 MPa) and supercritical (380 °C, 22.3 MPa) water containing 3.5 wt% NaCl and 3.0 wt% H<sub>2</sub>O<sub>2</sub> for up to 300 h. Scanning electron microscopy/energy-dispersive X-ray spectroscopy (SEM/EDS) analysis revealed that LR effectively densified the coating surface and enhanced its structural integrity. Corrosion assessments based on weight change, SEM, EDS, and X-ray computed tomography (CT) indicated that the TC4 coating significantly improved the corrosion resistance of 316 L SS by inhibiting the outward diffusion of metallic elements and the inward diffusion of oxygen. X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) analyses showed that the oxide film formed on the TC4 coating consisted mainly of Ti, Al, Fe, and Cr oxides, and the inhibition effect of the coating on the matrix elements varied after different treatment processes. In particular, the 0.6 mm laser-enhanced coating has a lower corrosion weight change, a more uniform and dense corrosion surface, and a better inhibition. The combination of CS and LR is demonstrated to be an effective approach for enhancing the corrosion resistance of 316 L SS, showing great potential for application in super/subcritical water oxidation reactors.</div></div>","PeriodicalId":17078,"journal":{"name":"Journal of Supercritical Fluids","volume":"229 ","pages":"Article 106804"},"PeriodicalIF":4.4,"publicationDate":"2025-10-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145322496","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
A novel delamination process for multilayer plastic films using supercritical CO₂ is proposed as a sustainable alternative to facilitate their recycling. The method involves exposing the films to pure CO2 or CO2 modified with a small amount of cosolvent under mild conditions (40–80 ºC, up to 200 bar), followed by rapid depressurisation. As proof of concept, the delamination of three commercial films used in food packaging is presented. The starting material and the delaminated layers were analysed by ATR-FTIR, TGA, DSC and SEM microscopy. Multilayer polymer films formed by polyethylene (PE) and polyethylene terephthalate (PET) or PE and Machine Directed Oriented PE (MDO-PE) prepared with polyurethane adhesive (PU) were delaminated at the PET/PU and MDO-PE/PU interfaces. Furthermore, PolyAl from an aseptic beverage carton delaminated partially, releasing a thin PE layer and an aluminium-enriched PolyAl composite. DMSO and methanol showed the highest delamination efficiency among the cosolvents, while acetone and water were ineffective under the conditions studied. A multiple mechanism for the process is proposed: (1) mechanical stress due to CO₂-induced polymer swelling and rapid depressurisation; (2) selective adhesive debonding via cosolvents. Further studies are needed to corroborate the mechanism, validate the process across varied materials, and optimise its performance. This technology could contribute significantly to a more circular and sustainable economy.
{"title":"Sustainable delamination of multilayer plastic films for advanced recycling","authors":"Ramiro J. Olmos-Greco , Eduardo Pérez , Lourdes Calvo , Albertina Cabañas","doi":"10.1016/j.supflu.2025.106813","DOIUrl":"10.1016/j.supflu.2025.106813","url":null,"abstract":"<div><div>A novel delamination process for multilayer plastic films using supercritical CO₂ is proposed as a sustainable alternative to facilitate their recycling. The method involves exposing the films to pure CO<sub>2</sub> or CO<sub>2</sub> modified with a small amount of cosolvent under mild conditions (40–80 ºC, up to 200 bar), followed by rapid depressurisation. As proof of concept, the delamination of three commercial films used in food packaging is presented. The starting material and the delaminated layers were analysed by ATR-FTIR, TGA, DSC and SEM microscopy. Multilayer polymer films formed by polyethylene (PE) and polyethylene terephthalate (PET) or PE and Machine Directed Oriented PE (MDO-PE) prepared with polyurethane adhesive (PU) were delaminated at the PET/PU and MDO-PE/PU interfaces. Furthermore, PolyAl from an aseptic beverage carton delaminated partially, releasing a thin PE layer and an aluminium-enriched PolyAl composite. DMSO and methanol showed the highest delamination efficiency among the cosolvents, while acetone and water were ineffective under the conditions studied. A multiple mechanism for the process is proposed: (1) mechanical stress due to CO₂-induced polymer swelling and rapid depressurisation; (2) selective adhesive debonding via cosolvents. Further studies are needed to corroborate the mechanism, validate the process across varied materials, and optimise its performance. This technology could contribute significantly to a more circular and sustainable economy.</div></div>","PeriodicalId":17078,"journal":{"name":"Journal of Supercritical Fluids","volume":"229 ","pages":"Article 106813"},"PeriodicalIF":4.4,"publicationDate":"2025-10-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145322499","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-10-10DOI: 10.1016/j.supflu.2025.106803
Junyang Li , Chiara Bufalini , Stefania Mottola , Maria Chiara Iannaco , Roberta Campardelli , Iolanda De Marco
Lycopene, a lipid-soluble carotenoid with potent antioxidant properties, is typically found in tomato peels, which are often discarded as by-products in the food industry. This study focused on extracting lycopene using solvent extraction and encapsulating it in polycaprolactone (PCL), a biodegradable polymer, using two different methods: solvent evaporation and supercritical emulsion extraction (SEE). Both methods were used to produce microparticles for nutraceutical applications. An optimization study based on Box-Behnken design and response surface modelling was conducted to assess the effects of emulsification stirring speed, emulsification time, and polymer amount on encapsulation efficiency and particle size. Particle sizes, measured by laser diffraction, ranged between 1.77 ± 0.10 and 2.82 ± 0.17 μm for solvent evaporation, and between 1.12 ± 0.03 and 2.72 ± 0.15 μm for SEE. Encapsulation efficiencies, measured by UV–vis spectroscopy, ranged between 28.45 ± 0.28 % and 89.94 ± 1.70 % for solvent evaporation, and between 66.52 ± 0.64 % and 89.45 ± 1.31 % for SEE. Results show that SEE yields more consistent encapsulation efficiencies compared to solvent evaporation. Additionally, the design of experiments (DoE) approach helped identify optimal conditions that minimize waste and maximize productivity. This work offers a sustainable method for converting agro-industrial waste into valuable nutraceutical products.
{"title":"Valorisation of tomato peel waste for lycopene encapsulation: Optimization and comparison of two green techniques","authors":"Junyang Li , Chiara Bufalini , Stefania Mottola , Maria Chiara Iannaco , Roberta Campardelli , Iolanda De Marco","doi":"10.1016/j.supflu.2025.106803","DOIUrl":"10.1016/j.supflu.2025.106803","url":null,"abstract":"<div><div>Lycopene, a lipid-soluble carotenoid with potent antioxidant properties, is typically found in tomato peels, which are often discarded as by-products in the food industry. This study focused on extracting lycopene using solvent extraction and encapsulating it in polycaprolactone (PCL), a biodegradable polymer, using two different methods: solvent evaporation and supercritical emulsion extraction (SEE). Both methods were used to produce microparticles for nutraceutical applications. An optimization study based on Box-Behnken design and response surface modelling was conducted to assess the effects of emulsification stirring speed, emulsification time, and polymer amount on encapsulation efficiency and particle size. Particle sizes, measured by laser diffraction, ranged between 1.77 ± 0.10 and 2.82 ± 0.17 μm for solvent evaporation, and between 1.12 ± 0.03 and 2.72 ± 0.15 μm for SEE. Encapsulation efficiencies, measured by UV–vis spectroscopy, ranged between 28.45 ± 0.28 % and 89.94 ± 1.70 % for solvent evaporation, and between 66.52 ± 0.64 % and 89.45 ± 1.31 % for SEE. Results show that SEE yields more consistent encapsulation efficiencies compared to solvent evaporation. Additionally, the design of experiments (DoE) approach helped identify optimal conditions that minimize waste and maximize productivity. This work offers a sustainable method for converting agro-industrial waste into valuable nutraceutical products.</div></div>","PeriodicalId":17078,"journal":{"name":"Journal of Supercritical Fluids","volume":"229 ","pages":"Article 106803"},"PeriodicalIF":4.4,"publicationDate":"2025-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145311775","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-10-09DOI: 10.1016/j.supflu.2025.106798
Akira Yoko , Mitsuru Sasaki , Tadafumi Adschiri
Hydrolysis reactions occurring under high-temperature compressed water, particularly near the critical point, are important for various organic and inorganic reaction applications. Earlier studies have examined solvent effects of hydrolysis reactions during metal oxide formation. The effectiveness of the Kirkwood equation for describing solvent effects has been reported. Distinguishing the reactant effects of water is important to treat kinetics data. Various hydrolysis reactions of organic compounds have been studied intensively for several decades. However, in terms of solvent effects, the analysis operation and the microscopic interpretation of the data have not been well established. For this study, the hydrolysis reactions of trehalose were examined specifically by comparing those of cellobiose and supercritical hydrothermal synthesis of metal oxides. Among the various aspects of water effects, the solvent effects described using the Kirkwood theory after considering the reactant effects were demonstrated effectively by the study findings.
{"title":"Solvent effects on kinetics of hydrolysis reactions in supercritical water","authors":"Akira Yoko , Mitsuru Sasaki , Tadafumi Adschiri","doi":"10.1016/j.supflu.2025.106798","DOIUrl":"10.1016/j.supflu.2025.106798","url":null,"abstract":"<div><div>Hydrolysis reactions occurring under high-temperature compressed water, particularly near the critical point, are important for various organic and inorganic reaction applications. Earlier studies have examined solvent effects of hydrolysis reactions during metal oxide formation. The effectiveness of the Kirkwood equation for describing solvent effects has been reported. Distinguishing the reactant effects of water is important to treat kinetics data. Various hydrolysis reactions of organic compounds have been studied intensively for several decades. However, in terms of solvent effects, the analysis operation and the microscopic interpretation of the data have not been well established. For this study, the hydrolysis reactions of trehalose were examined specifically by comparing those of cellobiose and supercritical hydrothermal synthesis of metal oxides. Among the various aspects of water effects, the solvent effects described using the Kirkwood theory after considering the reactant effects were demonstrated effectively by the study findings.</div></div>","PeriodicalId":17078,"journal":{"name":"Journal of Supercritical Fluids","volume":"229 ","pages":"Article 106798"},"PeriodicalIF":4.4,"publicationDate":"2025-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145364353","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-10-06DOI: 10.1016/j.supflu.2025.106801
Minxing Zhang , Lidia Montero , Jose A. Mendiola , Elena Ibáñez
Ilex guayusa, a traditional Amazonian plant rich in caffeine and polyphenols, has attracted interest for its antioxidant and neuroprotective properties. This study evaluates the potential of green compressed fluid extraction techniques to recover bioactive compounds from I. guayusa leaves using environmentally friendly solvents: pressurized liquid extraction (PLE), gas-expanded liquids (GXL), and supercritical fluid extraction (SFE). A mixture design approach combining CO2, ethanol, water, and 2-methyltetrahydrofuran (2-MTHF) in different proportions as solvents was applied to optimize extraction conditions. Among the tested methods, GXL extraction yielded the highest phenolic content and demonstrated superior antioxidant (ABTS and DPPH) and anti-inflammatory (inhibition of lipoxigenase, LOX) activities. Conventional water maceration showed stronger cholinesterase inhibition, suggesting complementary neuroprotective potential. Chemical profiling (HPLC-DAD-ESI-MS/MS) of the optimized extract confirmed the presence of phenolic acids and flavonoids associated with the observed bioactivities. These findings highlight the effectiveness of compressed fluid-based green extraction for obtaining multifunctional phytochemicals from I. guayusa, with promising applications in functional foods and nutraceuticals.
{"title":"Towards sustainable extraction of bioactive compounds from guayusa (Ilex guayusa): A comparative study on compressed fluids’ performance","authors":"Minxing Zhang , Lidia Montero , Jose A. Mendiola , Elena Ibáñez","doi":"10.1016/j.supflu.2025.106801","DOIUrl":"10.1016/j.supflu.2025.106801","url":null,"abstract":"<div><div><em>Ilex guayusa</em>, a traditional Amazonian plant rich in caffeine and polyphenols, has attracted interest for its antioxidant and neuroprotective properties. This study evaluates the potential of green compressed fluid extraction techniques to recover bioactive compounds from <em>I. guayusa</em> leaves using environmentally friendly solvents: pressurized liquid extraction (PLE), gas-expanded liquids (GXL), and supercritical fluid extraction (SFE). A mixture design approach combining CO2, ethanol, water, and 2-methyltetrahydrofuran (2-MTHF) in different proportions as solvents was applied to optimize extraction conditions. Among the tested methods, GXL extraction yielded the highest phenolic content and demonstrated superior antioxidant (ABTS and DPPH) and anti-inflammatory (inhibition of lipoxigenase, LOX) activities. Conventional water maceration showed stronger cholinesterase inhibition, suggesting complementary neuroprotective potential. Chemical profiling (HPLC-DAD-ESI-MS/MS) of the optimized extract confirmed the presence of phenolic acids and flavonoids associated with the observed bioactivities. These findings highlight the effectiveness of compressed fluid-based green extraction for obtaining multifunctional phytochemicals from <em>I. guayusa</em>, with promising applications in functional foods and nutraceuticals.</div></div>","PeriodicalId":17078,"journal":{"name":"Journal of Supercritical Fluids","volume":"229 ","pages":"Article 106801"},"PeriodicalIF":4.4,"publicationDate":"2025-10-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145271493","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-10-03DOI: 10.1016/j.supflu.2025.106802
Daichi Imai, Ikuo Ushiki
This study presents the first investigation of the equilibrium adsorption of 1-butanol on activated carbon in a supercritical CO2 environment, covering a temperature range of 313 K to 353 K and pressures from 10.0 MPa to 20.0 MPa. A fixed-bed column setup, combined with flame ionization detection, enabled the accurate quantification of equilibrium adsorption in supercritical CO2. The Dubinin–Astakhov (DA) equation was used to model the equilibrium data and derive physically meaningful parameters: EVOC (interaction energy between VOC and adsorbent) and W0,VOC (saturated adsorption volume). Among the alcohol-based VOCs tested, 1-butanol consistently showed the strongest affinity for the activated carbon surface, due to its molecular structure and lower volatility. In addition to confirming common trends such as the effect of CO2 density on adsorption capacity, this study uniquely shows that adsorption energy increases systematically with VOC molecular size, and that saturated adsorption volume is inversely related to saturated fugacity of VOCs. These findings offer a new thermodynamic perspective that links microscopic molecular properties to macroscopic adsorption behavior, thereby enhancing our understanding of VOC adsorption under supercritical CO2 conditions.
{"title":"1-butanol adsorption on activated carbon in supercritical CO2: Experimental measurements and thermodynamic modeling","authors":"Daichi Imai, Ikuo Ushiki","doi":"10.1016/j.supflu.2025.106802","DOIUrl":"10.1016/j.supflu.2025.106802","url":null,"abstract":"<div><div>This study presents the first investigation of the equilibrium adsorption of 1-butanol on activated carbon in a supercritical CO<sub>2</sub> environment, covering a temperature range of 313 K to 353 K and pressures from 10.0 MPa to 20.0 MPa. A fixed-bed column setup, combined with flame ionization detection, enabled the accurate quantification of equilibrium adsorption in supercritical CO<sub>2</sub>. The Dubinin–Astakhov (DA) equation was used to model the equilibrium data and derive physically meaningful parameters: <em>E</em><sub>VOC</sub> (interaction energy between VOC and adsorbent) and <em>W</em><sub>0,VOC</sub> (saturated adsorption volume). Among the alcohol-based VOCs tested, 1-butanol consistently showed the strongest affinity for the activated carbon surface, due to its molecular structure and lower volatility. In addition to confirming common trends such as the effect of CO<sub>2</sub> density on adsorption capacity, this study uniquely shows that adsorption energy increases systematically with VOC molecular size, and that saturated adsorption volume is inversely related to saturated fugacity of VOCs. These findings offer a new thermodynamic perspective that links microscopic molecular properties to macroscopic adsorption behavior, thereby enhancing our understanding of VOC adsorption under supercritical CO<sub>2</sub> conditions.</div></div>","PeriodicalId":17078,"journal":{"name":"Journal of Supercritical Fluids","volume":"229 ","pages":"Article 106802"},"PeriodicalIF":4.4,"publicationDate":"2025-10-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145236640","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}