Tetra pak packaging is one of the most frequently used types of packaging in the food industry. The recycling of the tetra pak packaging waste presents a difficult task because of its multi-layered, multi-component structure. In this study, the degradation of tetra pak packaging in subcritical (SubCW) and supercritical (SCW) water was investigated. The experiments were carried out in one (SCW) or two stages (SubCW and SCW), whereby the influence of the reaction temperature and time on the yield and composition of the products obtained was investigated. The maximum oil phase yield achieved in a one-stage and a two-stage degradation process was 60.7% and 65.5%, respectively. The oil and gas phases were composed of different types of hydrocarbons. Higher temperature and longer time led to higher amounts of saturated aliphatic hydrocarbons in both the oil and gas phases. The aqueous phase contained sugars (glucose, fructose) and sugar derivatives (levulinic acid, glyceraldehyde, furfurals). Based on these results, the degradation pathway of waste tetra pak packaging in SubCW and SCW was proposed. The results of the study show that the degradation of waste tetra pak packaging with SubCW and SCW is a promising recycling process.

Gelidium sesquipedale is valued in the Spanish agar industry, but its production generates substantial waste, often discarded despite its nutritional and bioactive content. Subcritical water extraction (SWE) at 175 °C and 50 bar for 130 min was performed on this waste after agar extraction, comparing it to conventional ethanol extraction. The SWE extract exhibited superior nutritional profile, including proteins (170.6 ± 1.0 mg/gfreeze-dried-extract), essential amino acids (18.1%), carbohydrates (148.1 ± 0.3 mg/gfreeze-dried-extract), total phenolic content (57 ± 7 mg-EqGA/gfreeze-dried-extract), and also containing Maillard reaction compounds, such as 5-hydroxymethylfurfural, furfural, 2-furanmethanol, 1-(2-furanyl)-ethanone, and 5-methyl-2-furfural, influencing color, aroma and flavor. This extract showed better antioxidant and anti-inflammatory properties than the conventional extract, and higher xanthine oxidase, tyrosinase, and acetylcholinesterase inhibition activities. Toxicological assessment on human cells indicated the safety of the SWE extract. Therefore, SWE technology offers a promising method to valorize G. sesquipedale residue, yielding a bioactive and nutrient-rich extract suitable for food and nutraceutical applications.

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.

A green strategy employing water as solvent has been adopted to obtain protein hydrolysates from fish meal (FM), its water-soluble fraction (WSP), and its non-water-soluble fraction (NSP). The techno-functional properties of the hydrolysates have been investigated and compared to hydrolysates obtained with Alcalase®. In general, SWH hydrolysates presented higher content of free amino acids and higher degree of hydrolysis, which reflected on the molecular size distribution. However, Alcalase® hydrolysates presented better solubility (from 74 ± 4% for NSP at pH = 2 up to 99 ± 1% for WSP at pH = 4-7). According to fluorescence experiments, FM and NSP hydrolysates showed the highest surface hydrophobicity, which has been related to better emulsifying properties and higher emulsion stability. The emulsions stabilized with 2%wt. of SWH-treated NSP showed the smallest particle sizes, with D[4,3] = 155 nm at day 0, and good stability, with D[4,3] = 220 nm at day 7, proving that water fractionation followed by SWH treatment is a good method to improve the techno-functional properties of the hydrolysates.

In order to broaden the application range of squash polysaccharide (WESP/SWESP) and caffeic acid (CAA) and improve the quality of potato starch (PS) products, the effects of WESP/SWESP and CAA on the gelatinization, rheology, thermodynamics, microstructure and in vitro digestion of PS were investigated. Meanwhile, the synergistic effect of WESP/SWESP and CAA on PS was further analyzed. Differently, due to WESP and SWESP had different monosaccharide composition and structure, they had different effects on the system. Pasting properties results showed that the presence of WESP/SWESP and CAA significantly reduced the peak viscosity, trough viscosity, breakdown viscosity and final viscosity of PS, especially under the combined action. In rheological tests, all sample gels belonged to the pseudoplastic fluids and weak gel system (tan δ < 1). Besides, thermodynamic properties revealed that WESP/SWESP and CAA synergistic effect had better retrogradation delay effect. In the ternary system, WESP/SWESP, CAA and PS can form a new network structure and improve the stability of the gel system. In addition, the results of infrared spectroscopy, Raman spectroscopy, x-ray diffraction and scanning electron microscopy exhibited that the ternary system can promote the accumulation and winding of the spiral structure of PS chain, and make the structure of PS gel network more orderly and stable. Furthermore, compared with PS gel, the ternary system had lower RDS and higher SDS and RS content, suggesting that the addition of WESP/SWESP and CAA at the same time was more conducive to reducing the hydrolysis rate of PS. This work revealed the interaction between WESP/SWESP, CAA and PS, which improved the physicochemical and digestive properties of PS. It will provide a theoretical basis for improving the quality of potato starch-related products and developing functional foods.

The effects of subcritical water microenvironment on the physiochemical properties, antioxidant activity and in vitro digestion of polysaccharides (SWESPs) from squash were investigated. After single-factor experiments, twenty samples were successfully prepared at different extraction temperatures (110, 130, 150, 170 and 190 °C) and extraction times (4, 8, 12 and 16 min). Under a low temperature environment, the whole process was mainly based on the extraction of SWESP. At this time, the color of SWESP was white or light gray and the molecular mass was high. When the temperature was 150 °C, since the extraction and degradation of SWESP reached equilibrium, the maximum extraction rate (18.67%) was reached at 150 °C (12 min). Compared with traditional methods, the yield of squash SWESP extracted by subcritical water was 3-4 times higher and less time consuming. Under high temperature conditions, SWESPs were degraded and their antioxidant capacity and viscosity were reduced. Meanwhile, Maillard and caramelization reactions turned the SWESPs yellow-brown and produced harmful substances. In addition, different SWESPs had different effects on in vitro digestion. In brief, SWESPs prepared under different conditions have different structures and physicochemical properties, allowing the obtainment of the required polysaccharide. Our results show that squash polysaccharides prepared in different subcritical water states had good development potential and application in the food industry.

Recovery of bioactive compounds from biowaste is gaining more and more interest in circular economy models. The oilseed cakes are usually insufficiently exploited by most technologies since they represent valuable matrices abundant in proteins, minerals, and phytochemicals, but their use is mostly limited to feed ingredients, fertilizers or biofuel production. This study was thus focused on the exploration of new valorization pathways of oilseed cakes by subcritical water, representing a safe and economic alternative in the creation of value chains. Pumpkin, hemp, and flax seed cakes were treated with subcritical water in nitrogen and carbon-dioxide atmospheres, as well as in nitrogen atmosphere with the addition of acid catalyst. The degradation of carbohydrate fraction was studied by quantifying sugars and sugar degradation products in the obtained extracts. The extracts obtained under different conditions were further compared chemically with respect to total phenols and flavonoids, as well as to the content of individual phenolic compounds. Furthermore, the effects of subcritical water treatment conditions on antioxidant, antiradical and cytotoxic properties of thus obtained extracts were defined and discussed.

Curcumin, a vital bioactive compound found naturally, has diverse biological applications. However, a major limitation of curcumin is its low bioavailability caused by its limited solubility in water. Hence, it is possible to overcome this problem through preparing oil in water nanodispersion of curcumin that emulsifier can play key role to produce nanodispersion. In the present study, the effect of three emulsifiers of Tween 80, Arabic Gum and Polyethylene glycol on preparing nanodispersions with desirable properties was investigated using subcritical water method and a mixture design. Zeta-potential and particle size of the achieved nanodispersions were taken into account as outcome factors. The optimum values for emulsifiers of Tween 80, Arabic Gum and Polyethylene glycol were obtained as 0.588 g, 0.639 g and 0.273 g, respectively, using the suggested model, so that obtained nanodispersion had minimum particle size (101.89 nm) and maximum zeta-potential (-24.99 mV). In fact, 102.5 nm and - 24.7 mV were obtained from experimental data at these values of emulsifiers. In addition, maximum loading potential (0.199 g/L), efficiency (99.5%), and minimum total curcumin loss (0.5%) were acquired at these optimum values. The results also show that the nanodispersion had a powerful antioxidant activity (65.27%) with extra antibacterial activity in facing with both E. coli and S. aureus strains. Moreover, curcumin nanodispersion was significantly taken up by HT-29 cells and resulted in the production of oxidative stress in the cells, leading to a decrease in the growth of cancer cells.

This study investigated the effects of subcritical water (SW) temperatures on the hydrolysis pattern and characteristics of hydrolysates prepared with strong rice (SR) and floury rice (FR). The characteristics of the hydrolysates were generally dependent on the rice cultivar in the SW temperature range of 150-250 °C, while the cultivar dependence was diminished at temperatures greater than 300 °C. Based on brix and reducing sugar content, an optimal production of rice hydrolysates was obtained at a SW temperature range of 200-250 °C. However, thermal conversion of sugar into acids, 5-hydroxymethylfurfural (HMF) and furfural was manifested at 250 °C. The rice hydrolysates prepared at 250 ∼ 300 °C had the highest antioxidant activity with strong umami intensity, but they suppressed the growth of prebiotics. Therefore, the present study demonstrated that controlling the SW temperature is crucial to improve rice hydrolysis efficiency and to regulate the physiological activity of the hydrolysates.

In this study, the polysaccharide from Glycyrrhiza inflata Batalin extracted by hot water (HW-GP) was further physically modified with subcritical water to obtain novel polysaccharides (SW-GP). Comparative analysis was conducted to examine the disparities in conformation and bioactivity between HW-GP and SW-GP, aiming to precisely regulate the structure of the polysaccharides and enhance their bioactivity by controlling subcritical water temperature. The results showed that, compared with HW-GP, subcritical water modification (100-160 °C) not only significantly reduced the molecular weight of polysaccharides (from 5.586 × 105 g/mol to 1.484 × 105 g/mol), but also modulated the intermolecular interaction forces, which maintain the conformation of the polysaccharides, including electrostatic and hydrophobic interactions, thereby dynamically transforming the polysaccharide chain conformation from triple helix to random coil, and the strength of the chain conformation shifted from rigid to flexible. In addition, the modification of the SW-GP structure by subcritical water also enhanced its biological activity. SW-GP (140 °C) with low molecular weight and semi-rigid triple helix conformation showed the best scavenging effect on the DPPH, ABTS, and hydroxyl radicals, and exhibited excellent antioxidant activity. SW-GP (130 °C) with medium molecular weight and semi-rigid triple helix conformation significantly promoted the proliferation and phagocytosis of RAW264.7 cells, as well as increased the release levels of NO, TNF-α, IL-6, and IL-1β, and the immunomodulatory activity was much higher than that of other polysaccharides. These findings confirmed the feasibility of using subcritical water temperature as a regulatory feature for the structure and bioactivity of glycyrrhiza polysaccharides, which may have reference significance for the modification of polysaccharides with heightened bioactivity.