Polysaccharides

The search for developing materials of natural origin has become imperative due to the resistance shown by phytopathogenic microorganisms to traditional antimicrobial agents. Natural polymers such as chitosan offer a new alternative to fungal infections because, in most cases, these polymers are biocompatible, nontoxic, and natural. This study aimed to synthesize nanochitosan using ultrasonication and evaluate its antifungal activity on Colletotrichum chrysophillum and Colletotrichum musae. Nanochitosan of 302.4 ± 92.3 nm and a zeta potential of +35.9 ± 2.3 Mv, amorphous in shape, and a rough surface, was obtained. Nanochitosan reduced the radial growth 21%, for C. chrysophillum while C. musae showed a maximum inhibition of 26% at a concentration of 1.5 mg mL⁻¹ of nanochitosan. C. musae was the species most affected, with a 38% increase in hyphal diameter to 12 h. Also, nanochitosan affected the integrity of the fungi cell walls, plasma membrane, and generated low oxidative stress level. Our findings indicate that nanochitosan induces notable changes in the intracellular structures of the tested phytopathogens. Nevertheless, additional investigations are required to clarify the mechanisms underlying adaptability or resistance in fungal strains that exhibit reduced sensitivity to this biopolymer. Full article

There are limited studies in the literature on the surface characterization of modified graphene and graphene oxide and the impact of these modified adsorbents on adsorption performance. In addition, the amine group essentially has a promising affinity for carbon dioxide (CO₂). Therefore, chitosan was used in this study to be grafted onto graphene and graphene oxide respectively. This study examines the effects of graphene, graphene oxide, and chitosan-modified graphene oxide thin films on the removal of carbon dioxide (CO₂). Thin films of graphene, graphene oxide, and their chitosan-modified counterparts were prepared via the methods of precipitation and grafting. The differences in the chemical structure, surface properties, and surface morphology of the films were evaluated, and their effect on the adsorption performance of CO₂ is discussed herein. The micrographs from a scanning electron microscope (SEM) show that the surface of graphene oxide appeared to be more porous than graphene, and the amount of grafted chitosan on graphene oxide is higher than that on graphene. An analysis of atomic force microscope (AFM) finds that the surface of chitosan-modified graphene oxide is rougher than that of chitosan-modified graphene. The results of energy-dispersive X-ray spectroscopy (EDS) spectra reveal that the composition of oxygen in graphene oxide is greater than that in graphene and confirm that the oxygen and nitrogen contents of chitosan-modified adsorbents are greater than those of the pristine materials. An analysis of Fourier-transform infrared spectroscopy (FTIR) shows that most of the oxygen-containing groups are reacted or covered by amide or amine groups due to modification with chitosan. The adsorption isotherms for CO₂ adsorbed by the prepared graphene and graphene oxide presented as type I, indicating great adsorption performance under low pressure. The appropriate amount of chitosan for modifying graphene oxide could be found based on the change in surface area. Although the breakthrough times and the thicknesses of the mass transfer regions for graphene oxide modified with 0.9% and 1.2% chitosan were similar, the modification of graphene oxide with 0.9% chitosan was appropriate in this study due to a significant decrease in surface area with 1.2% chitosan dosage. The adsorption uptake difference between chitosan-modified graphene oxide and graphene was greater than that without modification with chitosan due to more chitosan grafted on graphene oxide. The Toth adsorption isotherm model was used to fit the adsorption uptake, and the average deviation was about 1.36%. Full article

Nowadays, agricultural biomass is one the most valuable sources of natural polysaccharides. In addition to primary agricultural goods, agricultural waste is abundant, diverse, and renewable and can also be utilized as raw material for the production of polysaccharides and their derivatives. The extraction and purification of agri-waste-derived polysaccharides involves multiple processes that can vary depending on the type of raw material and the specific polysaccharides targeted. This study proposes a particular pathway from corn waste to hemicellulosic polysaccharides, which involves alkaline treatment and several physicochemical separation/purification phases using precipitation and ion exchange resins (Purolite A400, Purolite A100+, Purolite C100H). The ion exchange separation stage was optimized to retain most of the acid-soluble lignin derivatives from the extraction liquors. The process parameters considered for optimization included the solid (resin) liquid (black liquor pH 4.5) ratio, contact time, and temperature. These ranged from 0.05 to 0.15 g·mL⁻¹, 30 to 180 min, and 20 to 50 °C, respectively. The chemical composition of the separated hemicelluloses varied from 44.43 to 75.28% for xylan, 2.43 to 3.93% for glucan, 1.86 to 2.44% for galactan and 8.93 to 12.68% for arabinan. The total carbohydrate content increased from 57.65 to 96.3%. Full article

Dyes abundance in industrial wastewater exerts adverse effects on the environment and human health; adsorption represents a promising remediation strategy. Chitosan-based composites are interesting materials for dye adsorption. In this work, methyl orange (MO) adsorption using chitosan (CH) and chitosan–graphene oxide (CH-GO) aerogels produced by supercritical gel drying, performed at 200 bar/35 °C, was assessed by studying the effect of driving force (25–100 ppm) and adsorbent dosage (1–8 g/L). It was highlighted that the difference in the performance between the two adsorbents was non-negligible only at high concentrations: processing a 100 ppm MO solution, q_eq is 59 mg/g and 28 mg/g for CH-GO and CH, respectively. Starting from a 10 ppm MO solution, using a dosage of 8 g/L, it was possible to achieve adsorption efficiency of about 85%, meaning that small amounts of nanostructured devices can result in good process outcomes. Freundlich isotherm reliably describes the system behavior (R² = 0.99). The multi-linear IPD kinetic model confirms that in the case of nanostructured porous devices, there are different mass transfer phenomena that control molecule diffusion through the system. The research proposed in this work aims to explore, as a first assessment, the potential of nanostructured devices for adsorption purposes. Full article

Xanthan gum (XG) is a well-known anionic polysaccharide that finds broad application in the food and petroleum industries because of its ability to enhance solution viscosity at low concentrations and moderate temperatures. The aim of this work was to use the solvation probe coumarin 153 (C153) to characterize changes in the xanthan gum (XG) solution microstructure as a function of XG concentration and temperature from the perspective of a dissolved solute molecule. We established the utility of C153 fluorescence to track solution changes for XG concentrations that span the transition region from a dilute to a semi-dilute solution, defined by the xanthan gum overlap concentration, C*~0.02 g/dL. The temperature was varied from 293 to 353 K to probe solution conditions wherein XG has been reported to undergo a structural change from helix to random coil conformation, the details of which are still under debate. While C153 fluorescence does not elucidate direct structural information, the emission response is a simple means by which changes in aqueous XG solution can be identified. C153 spectroscopy is observed to correlate with XG conformational changes, as reported in the literature. Full article

Large quantities of seeds are generated and discarded during agro-industrial mango processing. However, mango seeds still contain valuable components such as starch, which has applications in various industries. This study aimed to obtain and characterize starches from the seeds of five mango cultivars (Ataulfo, Manililla, Piña, Tapana, and Tommy Atkins). The isolated starches were evaluated for their physicochemical, morphological, structural, thermal, and rheological characteristics. The starches showed creamy white colorations, and their granules had spherical and oval shapes. This starch source contains a high percentage of apparent amylose, greatly influencing its thermal, rheological, and functional properties. Structural and molecular studies showed that all starches presented an A-type X-ray diffraction pattern, impacting their water absorption and viscosity. The transition temperatures were relatively high, which could be influenced by the length of the amylopectin chains and their intermediate components, the apparent amylose content, and other components such as lipids and anomalous amylopectin. The starches evaluated behaved as pseudoplastic materials, while oscillatory tests revealed that the pastes formed with mango starches are more elastic than viscous. In conclusion, research on the seed starch properties of different mango cultivars provides interesting results for their potential application in foods. It could contribute to the value-added processing of mango seeds as a potential starch source. Full article

Bacterial cellulose (BC) is a versatile biopolymer with significant potential across biomedical, food, and industrial applications. To remove bacterial contaminants, such as protein and DNA, BC pellicles undergo purification, which traditionally relies on harsh alkali treatments, such as sodium hydroxide or strong surfactants, which present environmental concerns. In response, this study evaluates the efficacy of various non-conventional surfactants—both non-biodegradable and biodegradable—as alternatives for BC purification. Among the surfactants tested, sodium cocoyl isethionate (SCI), a mild anionic and biodegradable surfactant, emerged as particularly effective, achieving an 80.7% reduction in protein content and a 65.19% reduction in double-stranded DNA (dsDNA) content relative to untreated samples. However, these advantages were not without additional challenges, such as the appearance of residual surfactants. Given SCI’s promising performance and biodegradability, it was further examined in two-step treatment protocols; additionally, sodium dodecyl sulfate (SDS) was also examined as a more traditional anionic surfactant as well as NaOH. For the two-step treatment protocol, BC pellicles were treated with one reagent for 3 h, followed by a second reagent for an additional 3 h. Notably, by using NaOH as the final step in the two-step treatment protocol, residual surfactant was not detected in the FTIR analysis. Overall, this work demonstrates that SCI, in addition to subsequent NaOH treatment, can be used as a surfactant-based approach for BC purification, representing a potential environmentally friendly alternative to traditional surfactant-based approaches for BC purification. Full article

Polyelectrolyte complexes (PECs) have gained increasing attention in recent decades due to their importance in various applications, such as water treatment and paper processing. These complexes are formed by mixtures of polycations (n+) and polyanions (n−), known as polyelectrolytes (PEs). In this study, a series of PECs were prepared with different molar charge ratios (n−/n+) using biopolymers such as chitosan (lch) and pectin (p) at pH 5, in addition to the synthetic polymer poly(ethylene alt maleic acid) (PEMA) at the same pH. Two types of chitosan—low molecular weight chitosan (lch) and high molecular weight chitosan (hch)—were used as polycations, and these were mixed with two types of pectin with either a high esterification degree (hp) or a low esterification degree (lp), as well as PEMA as polyanions. These components interacted via electrostatic forces to form the following PEC combinations: (lch&lp), (lch&hp), (hch&hp), and (lch&PEMA). The charge density, turbidity, and particle size of the formed PECs were examined to evaluate the influence of molecular weight and mixing speed on the formation process. Full article

Here, super porous carboxymethyl cellulose (CMC) cryogels were synthesized in 10–100% crosslinker and the presence of TA, at varying amounts of TA, e.g., 10 and 25 wt% of CMC under cryogenic conditions (−20 °C) as TA@CMCs. To control the degradation of CMC cryogel networks, the crosslinking ratio of divinyl sulfone (DVS:X) to CMC varied at 10, 25, 50, and 100% moles of the CMC repeating unit. Higher hydrolytic degradation was observed for CMC 10%X cryogels at pH 1.0 with 28.4 ± 1.2% weight loss. On the other hand, the TA-release studies from TA@CMC-based cryogels showed that higher TA releases were observed for both TA@CMC 10% and 25% cryogels at pH 7.4, with 23.6 ± 1.1, and 46.5 ± 2.3 mg/g in 480 min, which are equal to almost 24% and 18% of the TA contents of the corresponding cryogels, respectively. The antioxidant properties of TA@CMC cryogels were examined, and worthy antioxidant properties were observed due to the TA. The alpha-glucosidase enzyme inhibition ability of the prepared cryogels was examined at different concentrations by grinding cryogels, and it was determined that TA@CMC 25% cryogel at 3 mg/mL concentration inhibited 70.4 + 1.3% of the enzyme. All bare CMC-based cryogels were found to be non-hemolytic with a less than 1% hemolysis ratio and also effective on the blood coagulation mechanism with blood-clotting index (BCI) values between 62.1 and 81.7% at 1 mg/mL concentrations. On the other hand, TA@CMC 25% cryogels exhibited a slight hemolytic profile with a 6.1 ± 0.8% hemolysis ratio and did not affect the blood coagulation mechanism with 97.8 ± 0.4% BCI value. Full article

PLA biocomposites, incorporating 5% wt. of lignocellulosic fibres (LF) from Posidonia oceanica waste with different degrees of cellulose purification, were obtained by melt blending and compression moulding. The LF were obtained after removing part of the non-cellulosic components by subcritical water extraction at 150 and 170 °C and after bleaching the extracted residues with hydrogen peroxide or sodium chlorite. The non-bleached LF provided the composites with a brown colour and opacity, while the bleached LF impacted the optical properties of composites to a lower extent, depending on their whiteness. The LF composition had a noticeable effect on the composites’ mechanical and barrier properties. All LF reduced the water vapour barrier capacity while promoting the oxygen barrier of the films. Bleached LF enhanced the film stiffness and reduced extensibility and resistance to break, whereas non-bleached LF had lower impacts on the tensile parameters. Considering the mechanical and barrier performance of the composites, the fibres obtained at 170 °C and bleached with sodium chlorite exhibited the best behaviour. Nevertheless, if transparency and colour are not limiting for the use of the films, untreated LF allowed for good preservation of the water vapour permeability of PLA films and enhanced the oxygen barrier capacity, with a similar mechanical response as the other non-bleached fractions. Full article

Cellulose nanomaterials have been demonstrated to be excellent barriers against grease, oxygen, and other vapors, but their implementation in packaging materials is challenging because of numerous technical and practical challenges. In this work, the oxygen, air, grease, and heptane barrier performance of copy papers coated with cellulose nanocrystals (CNCs), oxidized cellulose nanofibrils (TOCNs), and carboxymethyl cellulose (CMC) weas examined. The effects of different materials and processing conditions were evaluated for their impacts on the resulting barrier properties. TOCN coatings demonstrated significantly better barrier properties than CNC and CMC coatings due to the long-range networked structure of TOCN suspensions eliciting enhanced film formation at the paper surface. Neat coatings of nanocellulose did not readily result in strong oxygen barriers, but the addition of CMC and/or an additional waterborne water barrier coating was found to result in oxygen barriers suitable for packaging applications (1 cm³/m²·day transmission at low humidity with a 10 g/m² coating). Cast films and thick coatings of CMC were good barriers to oxygen, grease, and air, and its addition to cellulose nanomaterial suspensions aided the coating process and reduced coating defects. In all cases, the incorporation of additional processing aids or coatings was necessary to achieve suitable barrier properties. However, maintaining the strong barrier properties of nanocellulose coatings after creasing remains challenging. Full article

In the quest for sustainable and efficient solutions for modern electronics, flexible electronic devices have garnered global attention due to their potential to revolutionize various technological applications. The manufacturing of these devices poses significant challenges, particularly regarding environmental sustainability and ease of production. A novel method employing direct inkjet printing of silver nanoparticle (npAg) ink onto cellulose nanocrystal (CNC) substrates is presented, offering a promising alternative to conventional methods. This study demonstrates the ability of CNCs to serve as a flexible and biodegradable substrate that does not require complex post-printing treatments to achieve adequate electrical performance. This method was implemented in the fabrication of an electrowetting-on-dielectric (EWOD) device, achieving circuit patterns with high resolutions and reduced resistances. The findings not only validate the use of CNCs in flexible electronic applications but also underscore the potential of advanced printing techniques to develop flexible electronics that are environmentally sustainable and technically feasible. Full article

Immobilized enzyme reactors (IMERs) are critical tools for developing novel oligosaccharides based on the enzymatic catalysis of polysaccharides. In this paper, a novel glucuronan lyase from Peteryoungia rosettiformans was produced, purified, and then immobilized on a CIM^® CDI disk for cleaving glucuronan. The results showed that around 63.6% of glycuronan lyases (800.9 μg) were immobilized on the disk. The V_max values of immobilized glucuronan lyases did not significantly change (56.9 ± 4.7 μM∙min⁻¹), while the K_m values (0.310 ± 0.075 g∙L⁻¹) increased by 2.5 times. It is worth noting that immobilized glucuronan lyases overcame the catalytic inhibition of free enzymes observed under high glucuronan concentrations (0.5–2 g∙L⁻¹). circumscribed central composite design (CCCD) and response surface methodology (RSM) showed that glucuronan concentration, flow rate, and reaction time significantly affected the yield of oligoglucuronans. The degree of polymerization (DP) of degraded glucuronan ranged from DP 2–8 according to the results obtained by high performance anion exchange chromatography coupled with a pulsed amperometric detector (HPAEC-PAD). The IMER retained 50.9% activity after running 2373 column volumes of glucuronan. Finally, this glucuronan lyase reactor was tentatively connected to an immobilized laccase reactor to depolymerize, and gallic acid (GA) was added to glucuronan. Approximately 8.5 mg of GA was added onto 1 g of initial glucuronan, and the GA–oligoglucuronan conjugates showed notable antioxidant activity. Full article

Although diglycidyl ethers of glycols (DEs)—FDA-approved reagents for biomedical applications—were considered unsuitable for the fabrication of chitosan (CH) hydrogels and cryogels, we have recently shown that CH cross-linking with DEs is possible, but its efficiency depends on the nature of the acid used to dissolve chitosan and pH. To elucidate the origin of the low efficiency of chitosan interactions with DEs in acetic acid solutions, we have put forward two hypotheses: (i) DEs are consumed in a side reaction with acetic acid; (ii) DE chain length strongly affects the probability of cross-linking. We then verified them using FT-IR spectroscopy, rheological measurements, and uniaxial compression tests. The formation of esters in acetic acid solutions was confirmed for ethylene glycol diglycidyl ether (EGDE) and poly(ethylene glycol) diglycidyl ether (PEGDE). By the 7th day of gelation at pH 5.5, the G’_HCl/G’_HAc ratio was 5.1 and 1.5 for EGDE and PEGDE, respectively, indicating that the loss of cross-linking efficiency in acetic acid solution was less pronounced for the long-chain cross-linker. Under conditions of cryotropic gelation, only weak cryogels were obtained from acetic acid solutions at a DE:CH molar ratio of 1:1, while stable cryogels were fabricated at a molar ratio of 1:20 from HCl solutions. Full article

We cross-linked unfractionated heparin (H) using epichlorohydrin (E), in the absence or presence of imidazole (I), using various ratios of H, E, and I substances. The objectives and goals were to use the reaction for the preparation of medical materials suitable for blood sample applications. Nuclear magnetic resonance indicated the involvement of an H-end sequence [H-(1→4)-β-D-GlcA-(1→3)-β-D-Gal-(1→3)-β-D-Gal-(1→4)-β-D-Xyl-α-Ser] in the linkage with the 2-hydroxypropyl bridge. The yields of the individual experiments were found to increase in the following ratios: 1H/1E/3I (24%) < 1H/1E/2I (32%) < 1H/3E (42%) < 1H/1E/1I (46%) < 1H/2E (64%) < 1H/1E (77%). According to size-exclusion chromatography with multiple-angle light scattering (SEC-MALS) analysis, the mass at the peak increased in the following order: H (9292 g/mol) < 1H/1E (9294 g/mol) < 1H/2E (9326 g/mol) < 1H/3E (9708 g/mol) < 1H/1E/2I (11,212 g/mol) < 1H/1E/3I (12,301 g/mol) < 1H/1E/1I (13,800 g/mol) and in the reverse order with the increase in amount of epichlorohydrin and imidazole, i.e., 1H/1E > 1H/2E > 1H/3E and 1H/1E/1I > 1H/1E/2I > 1H/1E/3I. X-ray diffraction revealed that all prepared films were amorphous. An evaluation of the surface morphology using atomic force microscopy (AFM) confirmed a relatively low films roughness (~0.9–3.6 nm). The surface reduced elastic modulus, determined by the PeakForce quantitative nanomechanical mapping (PF-QNM) technique, was found to increase by up to ~63% for films cross-linked with E in the absence of I when compared with the results for the H substrate. A negligible change in modulus was, however, observed for films cross-linked in the presence of I, or was even reduced by ~15% (1H/1E/3I) compared to that for the H substrate. This could be explained by the parallel cross-linking of H only with E within its serine end unit and in competition with only one nitrogen of I. According to the highest yield (77%) of 1H/1E, the preferred product is the following: H-(1→4)-β-D-GlcA-(1→3)-β-D-Gal-(1→3)-β-D-Gal-(1→4)-β-D-Xyl-α-Ser-CH₂-CH(OH)-CH₂-OH. For the 1H/1E/1I (46% yield), 1H/1E/2I (32%), and 1H/1E/3I (24%) products, the cross-linked motif was the same, and the difference represented the surplus amount of the imidazolium cation ionically bound to the heparin anionic groups. Full article

Numerous bacterial species can both suppress plant pathogens and promote plant growth. By combining these bacteria with stabilizing substances, we can develop biological products with an extended shelf life, contributing to sustainable agriculture. Bacillus subtilis is one such bacterial species, possessing traits that enhance plant growth and offer effective protection, making it suitable for various applications. In this study, we successfully incorporated B. subtilis into hybrid materials composed of poly(3-hydroxybutyrate) (PHB) fibers coated with chitosan film. The polymer carrier not only supports the normal growth of the bioagent but also preserves its viability during long-term storage. For that reason, the impact of chitosan molecular weight on the dynamic viscosity of the solutions used for film formation, as well as the resulting film’s morphology, mechanical properties, and quantity of incorporated B. subtilis, along with their growth dynamics was investigated. SEM was used to examine the morphology of B. subtilis, electrospun PHB, and PHB mats coated with chitosan/B. subtilis. The results from mechanical tests demonstrate that chitosan film formation enhanced the tensile strength of the tested materials. Microbiological tests confirmed that the bacteria incorporated into the hybrid materials grow normally. The conducted viability tests demonstrate that the bacteria incorporated within the electrospun materials remained viable both after incorporation and following 90 days of storage. Moreover, the prepared biohybrid materials effectively inhibited the growth of the plant pathogenic strain Alternaria. Thus, the study provides more efficient and sustainable agricultural solutions by reducing reliance on synthetic materials and enhancing environmental compatibility through the development of advanced biomaterials capable of delivering active biocontrol agents. Full article

The increasing demand for sustainable materials has propelled research into polysaccharide modifications for various applications, particularly in active packaging. This review aims to explore the incorporation of bioactive compounds such as polyphenols into polysaccharides, focusing on chemical modification through free radical grafting techniques. The methods examined include enzymatic, physical, and chemical grafting techniques, highlighting their effectiveness in enhancing the properties of polysaccharide-based films. Recent studies have demonstrated that free radical grafting can significantly improve the mechanical, barrier, and antimicrobial properties of these films, extending their applicability in the food and pharmaceutical industries. However, challenges such as the stability of polyphenols and the understanding of grafting mechanisms remain critical areas for further investigation. This review discusses these advancements and outlines future research directions, emphasizing the potential of polysaccharide modifications to create innovative materials that meet the evolving needs of consumers and industries alike. Full article

The increasing production of plastics, driven by modern societal development, has resulted in a significant rise in plastic waste, which poses serious environmental concerns due to its lengthy degradation times. The growing issue of single-use plastics (SUPs), such as packaging for food items and disposable utensils, has led to their reduction and potential future prohibition in the European Union. Cellulose, a natural biopolymer sourced from nature, has been proposed as a viable alternative to SUPs because it degrades without toxicity. However, its limited barrier properties against water and grease have restricted its effectiveness as a substitute. This study focuses on developing an environmentally friendly alternative to SUPs by combining cellulose with acetylated starch and incorporating inorganic fillers like kaolin and talc. These fillers enhance the material’s barrier properties and reduce production costs. The results indicate that the addition of kaolin significantly lowers moisture absorption and water vapor permeability, while a mixture of kaolin and talc provides superior grease resistance. Additionally, incorporating D-sorbitol as a plasticizer improves the mechanical properties of the coated sheets, preventing cracking and enhancing strength. Overall, these coatings offer a promising alternative for packaging applications, such as for sugar, candies, or chocolate. Full article

Polysaccharide-functionalized gold nanoparticles (Au NPs) exhibit a promising application in biomedical fields due to their excellent stability and functional properties. The Au NPs from Auricularia auricula polysaccharide (AAP) were successfully synthesized using a straightforward method. By controlling the mass fraction of AAP, pH, reaction temperature, reaction time, and concentration of gold precursor, the highly dispersed spherical AAP-functionalized Au NPs (AAP-Au NPs) were prepared. The Fourier transform infrared spectrometer (FT-IR) and X-ray photoelectron spectroscopy (XPS) indicated that the synthesis mechanism of AAP-Au NPs was as follows: the molecular chain of AAP undergoes a glycosidic bond breakage to expose the reduction terminus in the presence of gold precursor, which reduced Au(III) to Au(0), and itself was oxidized to carboxylate compounds for maintaining the stability of AAP-Au NPs. Additionally, based on the electrostatic interactions and steric forces, as-prepared AAP-Au NPs exhibit excellent stability at various pH (5–11), temperature (25–60 °C), 5 mmol/L glutathione, and 0.1 mol/L Na⁺ and K⁺ solutions. Furthermore, AAP-Au NPs retained the ability to scavenge DDPH and ABTS radicals, which is expected to expand the application of Au NPs in biomedical fields. Full article