Polysaccharides

To increase the agricultural productivity in severely water-constrained areas affecting about one-sixth of the world’s population the development of effective and environmentally friendly superabsorbent hydrogels is imperative. This study aims to develop superabsorbent hydrogels based on two naturally derived components, quaternized chitosan (QCS) and montmorillonite (MMT) clay. Positively charged QCS interacts strongly with negatively charged MMT, leading to clay exfoliation, as was demonstrated by X-ray powder diffraction, infrared spectroscopy, thermogravimetric analysis and field-emission scanning electron microscopy coupled with energy dispersive X-ray spectroscopy. The potential of QCS/MMT gels for use in agriculture was verified through measurements of their swelling ability, mechanical properties, and water retention. It was shown that these gels can absorb up to 200 times their own weight in water. MMT particles were found to provide a two-fold increase in the Young’s modulus of hydrogels, which can help them withstand the pressure from surrounding soil particles during swelling inside the soil. As was shown by water retention studies on gel/sand mixtures, this leads to an enhanced water holding capacity and an increased water range available for plants for MMT-containing gels compared to pristine QCS gels. These findings are valuable for the research and development of bio-based superabsorbents for agricultural applications. Full article

This study reports the environmentally friendly synthesis of silver nanoparticles (LBP-AgNPs) using polysaccharides extracted from Lycium barbarum L. leaves as reducing agents. The synthesis was conducted through a green chemistry approach, eliminating the need for toxic chemicals. The structural properties of LBP-AgNPs were analyzed using a combination of UV-visible spectroscopy, Fourier-transform infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and atomic force microscopy (AFM). These techniques confirmed that the nanoparticles were well-dispersed, monodisperse, and crystalline, with sizes ranging from 10 to 80 nm. Additionally, the antioxidant activities of LBP-AgNPs were evaluated using DPPH and ABTS⁺ radical scavenging assays, which demonstrated significant free radical inhibition. The results suggest that LBP-AgNPs hold promise for various biomedical applications, including drug delivery, wound healing, and antioxidant therapies. Full article

Despite the established clinical benefits of insoluble dietary fibers (IDF), a significant “fiber gap” persists because their inclusion often conflicts with consumer sensory expectations. While general research on dietary fibers is abundant, few studies have systematically isolated the specific impacts of individual components on food quality. To maintain scientific accuracy, we explicitly acknowledge that because the primary literature predominantly evaluates raw agro-industrial by-products (e.g., brans, pomaces, hulls) rather than isolated, chemically pure polymers, a direct, isolated causal relationship to cellulose, hemicellulose, or lignin alone is often confounded by other matrix components. Our framework thus represents a synthesis of the dominant, most plausible roles of these polymers based on converging indirect evidence, rather than causal claims tested on pure substrates. This review characterizes these components through the “Backbone–Matrix–Cement” model to understand their distinct roles in food sensory science. Following PRISMA 2020 guidelines, a systematic search was conducted across ScienceDirect, Web of Science, Google Scholar, and PubMed. The review synthesized data from 106 sources, with 80.2% (85/106) published in the last five years (2020–2026). Data extraction included fiber type, food matrix, and analytical methods, with results grouped thematically. Cellulose (the Backbone) is crystalline, providing mechanical strength and structural stability; it is naturally white and flavor-neutral, primarily influencing firmness and hardness. Hemicellulose (the Matrix) has a high capacity for hydration and acts as a gelling medium. It improves moisture retention and softness in products like bakery goods. Lignin (the Cement) is a rigid, hydrophobic aromatic polymer that is most detrimental to palatability. It consistently causes darkening, bitterness, and astringency. The “coarse granular sensation” or gritty mouthfeel emerged as the primary barrier to consumer acceptance, largely driven by lignin and large cellulose particles. To mitigate these drawbacks, the review identifies several technological interventions: mechanical micronization, biological modifications (such as sourdough fermentation and enzymatic treatments), and chemical modifications (including ozonation and carboxymethylation). For optimal acceptance, formulation levels should generally remain below 10% in bakery products, keeping average particle sizes below the 150–200 µm threshold. Successful development of high-fiber functional foods requires targeted processing strategies that address the specific sensory liabilities of each component while maintaining nutritional efficacy. Full article

Natural functional polysaccharides are biodegradable, safe, and bioactive macromolecules that contribute significantly to food security. This review provides a systematic overview of their classification, structural characteristics, and applications in agricultural pest control and grain storage, with emphasis on their mechanisms of action and preparation methods. Key representatives including chitosan, alginate, β-glucan, and pectin function through multiple pathways: direct pest inhibition, induction of plant resistance, bioactive encapsulation, and physical barrier formation. Recent advances in extraction, purification, and advanced nuclear magnetic resonance (NMR) techniques—quantitative NMR (qNMR), diffusion-ordered spectroscopy (DOSY), and pure shift methods—are summarized. Challenges including batch-to-batch variability, high production costs, and regulatory hurdles are discussed and future perspectives on green production, precision structural tailoring, and nano-encapsulation are proposed. This review aims to guide the application of polysaccharide-based materials in insect pest management and food protection. Full article

Oxalis tuberosa (oca) is an underutilized Andean tuber with potential as an alternative starch source. This study compared native starches isolated from locally recognized yellow, pink, and black oca materials using compositional, structural, morphological, hydration, pasting, and thermal analyses. All starches exhibited B-type crystallinity but differed significantly in their measured characteristics. Black oca starch had the highest amylose content (28.1%), relative crystallinity (35.8%), median granule diameter (22.8 μm), and FTIR 1047/1022 ratio (1.36). Conversely, pink starch showed the highest swelling power at 90 °C (17.5 g g⁻¹), peak viscosity (3900 cP), and gelatinization enthalpy (12.83 J g⁻¹), compared with 10.9 g g⁻¹, 2350 cP, and 7.61 J g⁻¹, respectively, for black starch. The ordering of DSC parameters did not parallel XRD-derived relative crystallinity, indicating that relative crystallinity alone did not explain the thermal behavior. The contrasting functional profiles suggest that pink starch warrants further evaluation for applications requiring high hydration and viscosity development, whereas the lower RVA breakdown of black starch may be advantageous where resistance to viscosity loss during heating and shear is required. These findings demonstrate starch-level variation among the three local oca materials; however, application performance requires formulation-level validation, and broader multi-location and multi-harvest studies are needed to establish the stability of these characteristics. Full article

Antibiotic resistance represents a pressing global health challenge, with polymyxins serving as one of the last lines of defense against multidrug-resistant Gram-negative pathogens. Among them, polymyxin B (PMB) has gained renewed attention; however, its clinical use is limited by systemic toxicity. This study developed porous maize starch microparticles with tunable structure and surface chemistry to modulate PMB loading and release. Porous normal maize starch (NMS) and high-amylose maize starch (HAMS) were prepared by enzymatic treatment and modified by 2,2,6,6-Tetramethylpiperidine-1-oxyl (TEMPO)-mediated oxidation to introduce anionic carboxyl groups for PMB binding. Structural characterization revealed distinct pore morphology and lamellar organization in NMS- and HAMS-derived microparticles, while oxidation increased surface charge without disrupting granular integrity. TEMPO oxidation substantially enhanced PMB loading, suggesting that electrostatic interactions between PMB and oxidized starch contributed to adsorption. In an enzyme-assisted in vitro release model, oxidized porous starches exhibited biphasic profiles, with an initial rapid release followed by a plateau, indicating heterogeneous PMB binding. Oxidized porous NMS (NMS-P-T) and oxidized porous HAMS (HAMS-P-T) showed more sustained PMB release than non-oxidized particles. PMB-loaded HAMS-P-T maintained prolonged antibacterial activity against Escherichia coli in vitro relative to NMS-based matrices. These findings demonstrate that structural modification and surface-charge influence PMB loading and release behavior in starch microparticles, enabling the design of starch-based antimicrobial peptide delivery systems. Full article

Amidation is widely used to tailor alginate properties, yet different carbodiimide-mediated coupling procedures have been reported without establishing whether the reaction sequence affects the resulting materials. Here, this methodological gap was addressed by modifying sodium alginate with 1,4-butanediamine, 1,6-hexanediamine, and cystamine using two alternative reaction sequences. Both routes produced materials with comparable structural and physicochemical properties, demonstrating that, under the conditions studied, the reaction outcome was not significantly affected by the order of reagent addition. Beyond this methodological finding, the resulting derivatives exhibited a distinctive combination of aqueous processability and water stability: alkaline treatment followed by neutralization yielded homogeneous aqueous systems, whereas subsequent drying produced water-insoluble films. This behavior enables functional additives to be incorporated during aqueous processing while providing stable matrices upon water exposure. To demonstrate the technological relevance of these properties, the materials were evaluated as seed coatings using Vigna radiata as a model system. The 1,6-hexanediamine derivative showed the highest persistence under simulated rainfall without impairing germination, while Zn incorporation demonstrated the ability of the coating to act as a micronutrient carrier. Overall, these findings provide new insights into alginate amidation and establish a versatile route toward water-processable, water-stable functional coatings. Full article

Soybean hulls, an abundant agro-industrial by-product, were valorized as a renewable cellulose source for nanocellulose production. Cellulose isolates were obtained by alkaline treatment followed by bleaching with sodium chlorite (NaClO₂) or hydrogen peroxide (H₂O₂) and subsequently used to produce cellulose nanocrystals (CNC) and TEMPO-oxidized cellulose nanofibrils (CNF). Process efficiency and the structural and rheological properties of the resulting nanocelluloses were systematically compared. Sodium chlorite bleaching removed lignin and hemicellulose more effectively than hydrogen peroxide treatment, yielding isolates with higher cellulose content. Consequently, CNC_NaClO2 exhibited greater aspect ratio, higher crystallinity, and improved network-forming ability. Their suspensions showed pronounced viscoelastic and thixotropic behavior (G′ > G″), whereas CNC_H2O2 displayed lower moduli and nearly Newtonian flow. CNF suspensions exhibited dominant elastic behavior and gel-like consistency regardless of bleaching method, although this effect was stronger for CNF_NaClO2 due to the formation of longer, more entangled fibrils. FTIR confirmed the high purity of all nanocelluloses, while negative surface charge ensured colloidal stability. Overall, bleaching chemistry governed nanocellulose morphology and rheological performance, enabling tailored functional properties. By maintaining a constant biomass source and identical nanostructure production conditions while varying exclusively the bleaching agent, this study implements a controlled-variable design that rigorously isolates the effect of bleaching treatment. This systematic comparative framework provides methodological robustness rarely achieved in previous studies, where differences in raw materials or processing conditions often confound interpretation. Full article

The influence of chitosan (CS) molecular weight on the interfacial architecture of Ti₃C₂T_x MXene (MX)/chitosan composites (CS/MX) was investigated using complementary spectroscopic and microscopic techniques. Two commercial chitosans with distinct molecular weights and degrees of deacetylation (DD) were evaluated, CS-1 (91 kDa, 73.05% DD) and CS-2 (153 kDa, 69.52% DD). Ti₃C₂T_x MXene was synthesized by selective etching of Ti₃AlC₂ and characterized by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), attenuated total reflectance Fourier-transform infrared spectroscopy (ATR-FTIR), and Raman spectroscopy. XPS and Raman analyses provided evidence for successful MXene formation through a 45.4% reduction in surface aluminum content, a substantial increase in fluorine-containing surface terminations, and the emergence of the characteristic A₁g(Ti,C) Raman mode at ~200 cm⁻¹. Composite membranes containing different MXene loadings (MX-25, MX-50, and MX-75) were prepared by vacuum-assisted filtration and characterized. Morphological and spectroscopic analyses revealed that the lower-molecular-weight chitosan promoted more effective intercalation between MXene layers, resulting in expanded accordion-like structures and greater surface accessibility. In contrast, the higher-molecular-weight chitosan formed a thicker polymer coating that partially encapsulated the MXene sheets. ATR-FTIR, Raman, and XPS results demonstrated that CS-MX composite formation was governed by non-covalent interactions, primarily electrostatic attraction between protonated chitosan –NH₃⁺ groups and negatively charged MXene surface terminations, reinforced by hydrogen bonding. These findings demonstrate that chitosan molecular weight is a key design parameter governing the interfacial architecture and surface accessibility of Ti₃C₂T_x-based composites. Full article

Medicinal and edible homologous plant polysaccharides (MEHPs) and edible and medicinal mushroom polysaccharides (EMMPs) have attracted increasing attention due to their favorable safety profiles and diverse biological activities. However, existing reviews have mainly focused on individual extraction approaches or specific biological functions, lacking an integrated perspective that connects extraction strategies, structural characteristics, modification techniques, and industrial applications. This review provides a comprehensive analysis of MEHPs and EMMPs by systematically summarizing conventional and advanced extraction technologies, including ultrasound-, microwave-, and enzyme-assisted extraction, alongside deep eutectic solvent, supercritical fluid, and emerging physically assisted methods. Particular emphasis is placed on extraction mechanisms, kinetic modeling, structural preservation, and artificial intelligence-assisted process optimization. Furthermore, recent advances in multi-technique structural characterization, chemical modification strategies, structure–activity relationships, and applications in functional foods, prebiotics, drug delivery, and health-related fields are discussed. Finally, this review highlights key challenges limiting industrial translation, including raw material variability, insufficient higher-order structural characterization, unclear structure–activity relationships, limited clinical evidence, and regulatory barriers. Future perspectives integrating intelligent manufacturing, sustainable processing, and advanced computational approaches are proposed to facilitate the high-value and sustainable development of MEHPs and EMMPs. Full article

In this study, alginate hydrogels (A) cross-linked with a mixture of calcium and europium ions (Ca+Eu)A were developed for the first time as potential carriers for the targeted delivery and sustained release of drugs to specific regions of the gastrointestinal tract. Comparative studies were conducted to investigate the effect of the cross-linking agent (Ca²⁺, Eu³⁺, or their mixture) on the physicochemical properties of alginate hydrogels and the release kinetics of metronidazole in media simulating different gastrointestinal environments. Rheological analysis demonstrated that (Ca+Eu)A hydrogels form mechanically robust, highly cross-linked networks. The hydrogels exhibited negligible swelling in an acidic medium (swelling ratio, SR ≈ 1–1.5 g/g); however, in PBS, calcium alginate (CaA) hydrogels swelled 7–8 times more (SR ≈ 42.5 g/g) than hydrogels cross-linked with Eu³⁺ ions or a Ca²⁺/Eu³⁺ mixture (SR = 5–8 g/g). Metronidazole was released 1.5–2 times faster from calcium-cross-linked hydrogels than from hydrogels cross-linked with Eu³⁺ ions or the mixed Ca²⁺/Eu³⁺ system, whereas (Ca+Eu)A hydrogels exhibited a more sustained and uniform release profile. These results demonstrate that the drug release kinetics can be tuned by adjusting the Ca²⁺/Eu³⁺ ratio during alginate cross-linking. Consequently, such hydrogels represent a promising platform for the targeted delivery and controlled release of therapeutic agents, particularly antibiotics, to specific regions of the gastrointestinal tract. Full article

Fish processing by-products represent an abundant source of valuable biomolecules that can be valorized through sustainable extraction approaches. In this work, cod backbone hydrolysates obtained by subcritical water hydrolysis were incorporated into chitosan-based films for potential food packaging applications. The hydrolysis residue, rich in minerals, particularly hydroxyapatite (HAp residue), was also incorporated into the films to maximize the utilization of all hydrolysis-derived fractions. The effects of hydrolysate and HAp residue incorporation on the properties of the films were evaluated. The hydrolysate incorporation significantly improved the tensile strength of the films (from 11.56 to 24.39 MPa) and reduced water vapor permeability (from 4.93 to 2.89 (×10⁻¹¹) mol.m.m⁻².s⁻¹.Pa⁻¹), suggesting the formation of a denser and cohesive polymer network. However, the films also exhibited increased swelling and solubility (22–29% and 231–561%, respectively). When adding HAp residue, the films showed lower visible light transmittance and higher opacity, demonstrating improved light barrier properties. The addition of HAp residue also reduced swelling capacity but increased water vapor permeability and decreased tensile strength, suggesting the formation of a more heterogeneous film structure. Overall, the results demonstrate that cod backbone hydrolysates can be an alternative additive to chitosan films to tailor their functional properties for food packaging applications. The incorporation of hydroxyapatite-rich residues contributes to the full valorization of fish processing by-products, supporting the development of sustainable and biodegradable functional materials within a circular economy approach. Full article

The selection of appropriate materials is a critical step in designing an ideal wound dressing. One of the primary objectives of an ideal wound dressing is the prevention of bacterial infections. In this work bovine gelatine (BGE)–chitosan (CS) wound dressing films supplemented with propolis (PE) which is a well-known anti-bacterial agent were prepared by using solvent casting technique. The structures of the wound dressing films were characterized by FTIR and optical microscopy. Also, physical properties of the films such as thickness, mass, water vapor transmission rate (WVTR), water absorption capacity, water content and dressing pH were determined. The water content of films incorporating propolis was found to range from 18.8% to 23%. The water absorption capacity of these films varied between 137% and 646%, while their WVTR was observed to be between 1228.12 and 1593.75 g/m²·day. Additionally, the pH values of the prepared films ranged from 5.86 to 7.34, aligning with the typical pH range of human skin. Furthermore, the antibacterial potential of the BGE-CS-PE films was preliminarily assessed using the agar disc diffusion method against Gram-positive (S. aureus, B. subtilis) and Gram-negative (S. Typhi, E. coli) microorganisms. The observed inhibition zones suggested the potential contribution of propolis incorporation to the antibacterial properties of the films. The combined physical properties and preliminary antibacterial observations of the prepared films indicate their potential for wound dressing applications. Full article

Water-based drilling fluid systems are gaining popularity for their environmental friendliness and low cost. These fluids are highly sensitive to products used to modify fluid properties and control fluid loss. Traditional additives like carboxymethyl cellulose (CMC) work well but come with environmental issues and high costs and alternatives from agricultural sources are being sought. The potential of using acetylated yam peel starch (AYPS) and acetylated plantain peel starch (APPS) as substitutes for CMC in water-based drilling mud formulation under ambient and simulated downhole conditions of 27 °C and 150 °C, respectively, was investigated. The peels of yams and plantain, starchy foods, were chemically modified through acetylation and added to the drilling mud formulation at proportions of 0.2–1.0 g. FTIR confirmed the success of the modification by the presence of characteristic bands of carbonyl (C=O) absorption at 1730–1750 cm⁻¹ and by the increase in C–O bands after the modification, which means that acetyl groups were successfully incorporated. The highest mud density recorded was 9.16 kg/m³ (ppg) with 1.0 g of additives, and the pH values ranged from 8.10 to 9.50, which is good for drilling operations. The plastic viscosity was found to be 4–7 cP at 27 °C and 3–6 cP at 150 °C for AYPS and APPS, respectively, which were lower than the CMC value but still retained viscosity at high temperature. The yield point values for the samples were 2–5 lb/100 ft² at 27 °C and 1–6 lb/100 ft² at 150 °C, which were slightly better for AYPS. Thermal aging did not significantly affect gel strength, which increased upon exposure to high-temperature conditions, especially at high additive concentrations, indicating that the rheological properties were preserved. Filtrate losses were 12–16.8 mL for AYPS and 12.5–17.2 mL for APPS under low-pressure, low-temperature conditions, which are similar to CMC (11–16 mL). APPS was the most effective filtrate-loss control of the modified starch systems under the HPHT conditions. Rheological modeling showed that shear-thinning behavior is predominant, and the Herschel–Bulkley and Casson models provided the best fits. In general, the acetylated yam and plantain peel starches have shown promising properties as alternatives for CMC for enhancing rheological properties and controlling fluid loss in water-based drilling fluids. Full article

The escalating volume of agricultural waste presents not only a significant environmental challenge but also a substantial opportunity for resource recovery within a circular bioeconomy. This study investigates the feasibility of extracting high-quality cellulose from two underutilized agricultural residues: flower stems and tomato stems. Raw materials were subjected to a multi-stage chemical pulping process involving alkaline treatment, acid treatment, and hydrogen peroxide bleaching in order to remove lignin, hemicellulose, and other impurities. The resulting cellulose samples were comprehensively characterized for their yield, purity (α-cellulose content), degree of polymerization (DP), chemical structure (FT-IR), crystallinity (XRD), and inorganic elemental composition. The results demonstrate that both feedstocks can yield cellulose with an α-cellulose content exceeding 91% and a DP greater than 600, meeting the stringent quality requirements for dissolving-grade pulp intended for such applications as textiles, composite additives and others products. Flower stems showed a higher pulping yield (26.8%) compared to tomato stems (13.7%), highlighting their greater potential. This work validates agricultural residues, particularly flower stems, as a viable and sustainable alternative to traditional wood sources for cellulose production, offering a pathway to mitigate waste and add value to agricultural supply chains. Full article

Cherry tomatoes are highly susceptible to Salmonella contamination during pre- and post-harvest handling, leading to foodborne illness outbreaks and significant economic losses. Edible coatings incorporating natural antimicrobials offer a promising alternative to conventional chemical treatments for enhancing food safety while maintaining produce quality. This study developed and evaluated a pectin-based edible coating enriched with zinc nanohydroxide-thymol nanohybrids (ZnNH-T) for controlling Salmonella contamination and extending shelf-life of cherry tomatoes. ZnNH-T nanohybrids were synthesized via precipitation, followed by thymol intercalation, and characterized by SEM. Four coating formulations were prepared: pectin alone (P), pectin-thymol (PT), pectin-ZnNH (PNH), and pectin-ZnNH-T (PNHT). Antibacterial activity of the four coatings was first screened in vitro by disc diffusion against six S. enterica serovars; three serovars (Typhimurium, Enteritidis, and Montevideo) showing a statistically significant, coating-dependent inhibition response were selected for the postharvest assay. Cherry tomatoes were coated and dip-inoculated with three Salmonella serotypes (Typhimurium, Enteritidis, and Montevideo) at approximately 10⁵ CFU/mL and stored at 25 °C for 12 days. Antimicrobial efficacy, antioxidant activity (ABTS assay), and physicochemical quality parameters (weight loss, color, pH, and total soluble solids) were evaluated. Zinc nanohydroxides were successfully synthesized, as observed in SEM morphology. ABTS radical scavenging activity of filmogenic solutions was highest for PT (92.4%) and moderate for PNHT (65.9%), while P and PNH showed minimal activity (20.1% and 17.8%, respectively). PNHT coating achieved an approximately 2-log CFU/g reduction in Salmonella populations compared to uncoated controls over 12 days of storage, demonstrating sustained antimicrobial efficacy. Coated tomatoes exhibited significantly reduced weight loss (8% for PNHT vs. 13% for control), better color retention, lycopene content, maintained firmness, and stable pH and TSS values compared to uncoated controls. The pectin-ZnNH-T coating system represents a novel multifunctional approach for enhancing cherry tomato safety and quality. The use of thymol from the layered hydroxide structure, combined with zinc ion antimicrobial effects, provides sustained pathogen reduction while maintaining desirable physicochemical properties. This natural, biodegradable coating technology has potential for commercial application in fresh produce preservation. Full article

Pullulan, a natural microbial polysaccharide composed of repeating maltotriose units, is widely explored as a candidate for advanced cell culture configurations, tissue engineering (TE), and regenerative medicine (RM). Due to its excellent biocompatibility, lack of immunogenicity, and structural flexibility, it serves as a versatile base material. Pristine pullulan exhibits high water solubility and lacks intrinsic signals for cell attachment and proliferation. However, the presence of nine reactive hydroxyl groups per repeating maltotriose unit enables extensive chemical functionalization to address these limitations. This review provides a comprehensive analysis of multi-functional design strategies used to tailor pullulan into distinct structural forms, such as hydrogels, porous scaffolds, electrospun fibrous membranes, thin films, 3D-printed scaffolds, and self-assembling nanosystems. Polymer blending, chemical modification, and crosslinking strategies are discussed in relation to scaffold microstructure, pore size, degradation rate, and mechanical properties. In addition, these structural and physicochemical properties are correlated with biological performance, including cell migration, proliferation, and differentiation. Pullulan-based materials are particularly suited for applications requiring extensive chemical tunability, such as injectable hydrogels, bioinks, and multifunctional delivery systems. However, their intrinsic bioinertness and limited mechanical strength generally require combination with complementary components to achieve effective cell adhesion and structural stability. Finally, current processing limitations and future strategies are discussed for translating pullulan-based systems into clinical applications. Full article

Croscarmellose sodium (CCS) is a crosslinked cellulose-based superdisintegrant, widely utilized to enhance the disintegration and dissolution behavior of drugs from pharmaceutical solid dosage forms. In the present study, CCS was synthesized through controlled crosslinking of sodium carboxymethyl cellulose (CMC) by one-step synthesis and optimized using Response Surface Methodology (RSM) based on the Box–Behnken Design (BBD). The effects of four independent variables, namely isopropyl alcohol (IPA) concentration (70–100% v/v), reaction time (2–4 h), reaction temperature (50–70 °C), and concentration of crosslinking agent (CLA) (glycolic acid used as the CLA) (10–20% w/w of CMC weight), on swelling index (SI) and water retention capacity (WRC) of synthesized CCS were systematically evaluated. A total of 29 experimental runs, each representing a unique combination of reaction conditions generated by a three-level Box–Behnken Design (BBD) using Design-Expert^® software, were conducted to synthesize CCS samples. SI and WRC of each synthesized CCS sample were subsequently measured and used to develop statistically validated predictive models and identify the optimal synthesis conditions. The successful formation of croscarmellose sodium was critically confirmed by Fourier Transform Infrared (FTIR) spectroscopy. Analysis of variance (ANOVA) demonstrated that the developed models were statistically significant, with good predictive capability for both swelling index and water retention responses. A quadratic model adequately described the swelling index (R² = 0.9041, adjusted R² = 0.8083, p < 0.0001), whereas a linear model was selected for WRC (R² = 0.6112, adjusted R² = 0.5463, p < 0.0001). Reaction time and CLA concentration exhibited substantial influence on the functional properties of the synthesized CCS compared to other factors. The optimized synthesis conditions were identified as 93.23% IPA concentration, 4 h reaction time, 70 °C reaction temperature, and 10% CLA concentration. Under these conditions, the predicted swelling index and water retention capacity were 7.529 mL/g and 443.85%, respectively. Response surface analysis further revealed significant interaction effects among the synthesis variables, particularly between IPA concentration and reaction time. The findings of this study demonstrate that RSM-BBD is an effective statistical approach for optimizing cellulose-based superdisintegrant synthesis and provide valuable insights into the structure–property relationships governing the hydration and swelling behavior of CCS. The optimized CCS synthesized in this research thus shows potential for application as a high-performance pharmaceutical superdisintegrant in immediate-release tablet formulations. Full article

This work is focused on understanding how the properties of chitosan-g-poly(N,N-diethylacrylamide-co-N,N-dimethylacrylamide) and chitosan-g-poly(N,N-diethylacrylamide-co-N-ethylacrylamide) copolymers are affected by varying their compositions. Poly(N,N-diethylacrylamide), PDEAm, is a thermosensitive polymer with a reversible coil-to-globule transition in aqueous solution near the human body temperature. The transition temperature can be tuned by varying the amount of two more hydrophilic units: N-ethylacrylamide (NEAm) or N,N-dimethylacrylamide (DMAm). While the former can participate in hydrogen bonding as a proton donor or acceptor, the latter is only an acceptor and a very-well-known hydrophilic unit with no phase transition. The gelation process was followed by rheological measurements, showing the general features of the chemical gelation and the formation of a strong gel. A reaction autoacceleration was observed, which is interpreted by the high viscosity of the reaction mixture due to the presence of chitosan, although a greater effect was found in NEAm copolymers due to the higher hydrogen-bonding capacity of NEAm. A relationship was found between the compositions of both copolymers, the strength of the hydrogels, and the calculated pore size. The pore sizes range from 32 to 18 nm. Thermogravimetric analysis of the hydrogels showed the typical decomposition stages of polyacrylamides. Neither the temperature of the maximum decomposition rate nor the weight loss associated displayed a clear trend with the copolymer composition. There was an increment in the equilibrium swelling values with the content of NEAm units (from 16 to almost 28 g water/g polymer), but the copolymers with DMAm remained unaffected (swelling values around 23 g water/g polymer). The hydrogen-bonding interaction affected the gelation process and swelling behavior of the hydrogels. This can be explained by the greater ability of NEAm to form hydrogen bonds compared to DMAm. Full article