Ultrasound-assisted extraction (UAE) of polyphenols from the brown seaweeds Ascophyllum nodosum leaves a solid phase where alginates can be extracted. This study characterizes alginates extracted after the UAE process, with and without an intermediate drying stage at different temperatures (50 and 90 °C) producing sequentially two bioactive compounds from a unique raw material. FT-IR and ¹H NMR analyses showed the high purity of alginates with features in the range of commercial alginates. Drying at high temperature decreased average block length and viscosity average molecular weight (M_v) of alginate from 428 to 133 kg/mol. Steady-shear curves (shear-thinning behaviour) and viscoelasticity (liquid like character) features depended clearly on M_v. Solutions of alginates with high M_v were more viscous and the elastic character was more relevant. Cox-Merz rule was only accomplished within the semi-dilute regimes of alginate concentration. Tested process conditions allow the production of alginates with different properties.

Seaweeds have gained considerable attention in recent years due to their potential health benefits and high contents of bioactive compounds. This review focuses on the exploration of seaweed’s health-promoting properties, with particular emphasis on phlorotannins, a class of bioactive compounds known for their antioxidant and antidiabetic properties. Various novel and ecofriendly extraction methods, including solid–liquid extraction, ultrasound-assisted extraction, and microwave-assisted extraction are examined for their effectiveness in isolating phlorotannins. The chemical structure and isolation of phlorotannins are discussed, along with methods for their characterization, such as spectrophotometry, nuclear magnetic resonance, Fourier transform infrared spectroscopy, and chromatography. Special attention is given to the antioxidant activity of phlorotannins. The inhibitory capacities of polyphenols, specifically phlorotannins from Ascophyllum nodosum against digestive enzymes, such as α-amylase and α-glucosidase, are explored. The results suggest that polyphenols from Ascophyllum nodosum seaweed hold significant potential as enzyme inhibitors, although the inhibitory activity may vary depending on the extraction conditions and the specific enzyme involved. In conclusion, seaweed exhibits great potential as a functional food ingredient for promoting health and preventing chronic diseases. Overall, this review aims to condense a comprehensive collection of high-yield, low-cost, and ecofriendly extraction methods for obtaining phlorotannins with remarkable antioxidant and antidiabetic capacities.

Aqueous extracts fromAscophyllum nodosumbrown edible seaweeds were obtained after continuous ultrasound-assisted extraction. The effect of sonication time (from 2 to 6 min), sonication amplitude (from 80 to 100%) and solvent-solid ratio (from 20 to 40 g water g⁻¹dried seaweed) on the extracts features was studied employing a Box-Behnken experimental design. Extracts were characterised by polyphenols, carbohydrate and uronic acid content. Response surface method (by means of a quadratic model) was successfully employed to relate chemical composition of extracts and operation conditions. Optimal experimental conditions were established to obtain maximal polyphenols content and several polyphenols-carbohydrates ratios together with the conditions that minimise energy consumption per extracted polyphenols amount relationship. Antioxidant capacities of extracts were measured employing different methods (DPPH, FRAP and ABTS). Positive linear correlations between antioxidant activity and total polyphenols content were established.

The effect of several blending procedures between Ascophyllum nodosum seaweed flour (AF) and corn starch (CS) on the interactions between polyphenols and starch was studied in this paper. These methods comprised the blending of AF with native starch (NT) with previously gelled starch gel (GL) and promoting the gelling of corn starch in the presence of AF (CGL). Different AF–CS (g/g) ratios (from 1:0.5 to 1:25) were studied. The liquid phase was chemically characterized by polyphenols (TPC) and carbohydrates content. The antioxidant activity of the liquid phase after achieving the solid–liquid equilibrium was determined by DPPH, ABTS, and FRAP methods. The solid phase was characterized by FT-IR and SEM techniques. The Halsey model successfully fitted the equilibrium TPC in liquid and polyphenols adsorbed/retained by the solid phase of tested systems. NT samples showed lower polyphenols sorption than gelled samples. The differences found between samples obtained with GL and CGL methods suggested different interactions between polyphenols and starch. Specifically, physisorption is predominant in the case of the GL method, and molecular trapping of polyphenols in the starch gel structure is relevant for the CGL method. Results allowed us to determine the enhancement of the retention of polyphenols to achieve starchy foods with high bioactivity.

Water desorption isotherms of three alginates with different structural features were determined at 25, 37, and 50°C. The Halsey model was selected to fit the equilibrium water sorption data. Differential and integral enthalpy and entropy were estimated for tested alginates. Optimal storage conditions of tested alginates (moisture content from 0.15 to 0.20 kg water/kg dry solid and relative humidity from 35% to 50%) were determined from the maximum and minimum integral enthalpy and entropy values, respectively. A model was proposed to estimate the water sorption isotherms of alginates based on the alginate monomers (mannuronate, M, and guluronate, G) at low water activity (<0.4). M fraction was mainly responsible for the hygroscopicity of alginates. Alginates with similar G fraction showed different hygroscopic features by the presence of more homopolymeric G blocks that could form helical structures at low moisture content, decreasing the water affinity.Practical applications: Determination of water sorption isotherms is fundamental to determine the optimal storage conditions at different temperatures. Their knowledge is essential for designing drying equipment, selecting adequately drying conditions (temperature and relative humidity of air) and drying time. Mathematical models are useful to estimate equilibrium moisture content in wide ranges of water activity and temperature. The thermodynamic study also provides valuable information about energy consumption and consequently operational costs. In this case, high content of mannuronate, M, increases the hygroscopic character of alginates, but the optimal moisture content of dried alginates to achieve maximum stability during storing varies in a narrow interval (0.15–0.20 kg water/kg dry solid).

The isolation and chemical characterization of phlorotannins has gained special attention in recent years due to their specific health-promoting benefits. Flow-cell ultrasound-assisted extraction (90 W/cm² of sonication power, 2 min of retention time and 20 g solvent/g algae of liquid–solid ratio) was carried out by using double-distilled water (WE) and acetone:water mixture (AWE) as extraction solvents. The AWE showed a higher total polyphenols content (TPC), carbohydrates (CHOs) and antioxidant activities than WE. However, when the WE was purified by using Amberlite XAD16 column, the purified WE (PWE) showed similar a TPC, decreased CHOs and increased antioxidant activity compared to WE. The oxidation of the PWE extract was evaluated under natural, forced and severe oxidation condition for 120 h. Only severe oxidation conditions were able to significantly reduce TPC and antioxidant activities. PWE was dialyzed (20, 10, 3.5 and 2 kDa). The main bioactive fraction of phlorotannins was obtained from 10 to 20 kDa. CHOs were distributed in fractions below 20 kDa. MALDI-TOF analysis was performed for PWE, PD20 and PD2 extracts to analyze the degree of polymerization of phlorotannins, which ranged from 4 to 17 phloroglucinol units/molecule. Fragmentation patterns allowed the proximate identification of several phlorotannins in Ascophyllum nodosum extracts.