Freeze-drying Process Research Articles

The Application of Mulberry Elements into a Novel Form of Easy-to-Prepare Dried Smoothie

The European market offers a variety of functional foods targeted at prediabetic and diabetic patients, with different approaches to reducing postprandial glucose levels. The utilization of white and black mulberry in new products could be an area of interest to many conscious consumers. The study aimed to design a novel form (dried) of easy-to-prepare product by applying nutritious mulberry in various proportions and creating an aesthetically appealing smoothie product with a distinctive taste profile. Such an easy-to-prepare form of smoothie was obtained by utilizing the freeze-drying process, while typical market smoothies are liquid. Sensory evaluations of the fresh, dried, and reconstructed smoothies and their basic characteristics were conducted. Moreover, antiradical tests (with ABTS+• and DPPH•), the phenolic compound profile (HPLC/PDA), and the L*a*b profile were analyzed. The results of the sensory evaluation tests were divided into two groups: Polish and foreign panelists. It was observed that mulberry-licorice drop-based smoothies were preferred fresh. Yet dried and reconstituted capsule-based smoothies were favored overall. Generally, both Polish and foreign panelists preferred lower concentrations of mulberry and licorice extracts (DB) in fresh smoothies, while in dried or reconstructed smoothie form, panelists scored higher (DC) and lower (DB) concentrations quite similarly (favored both concentrations). From the group of identified phenolic compounds, cinnamic acid derivates dominated all analyzed smoothies. Many analyzed types of flavonoids (quercetin, rutin, kaempferol) and naringenin were found in the smoothies. Some differences were noted in the antiradical tests but were only statistically significant for DPPH• scavenging activity, which was higher for the DB1, DB2, and DC1 samples. Generally, even higher addition of licorice and mulberry did not negatively affect panelists’ ratings and the analyzed activities.

Comparison Between Simple Batch and Fed-Batch Bioreactor Cultivation of Recombinant BCG

Background/Objectives: Tuberculosis continues to be a significant global health concern, causing 1.3 million deaths in 2022, particularly affecting children under 5 years old. The Bacillus Calmette-Guérin (BCG) vaccine, developed in 1921, remains the primary defense against tuberculosis but requires modernized production methods. The recombinant BCG-pertussis strain shows potential in providing dual protection against tuberculosis and whooping cough, especially for vulnerable newborns, and enhanced efficacy against bladder cancer. Implementing submerged cultivation techniques for rBCG-pertussis production can offer increased productivity and standardization. Methods: This study explores a fed-batch cultivation strategy with pH-stat control to feed L-glutamic acid through the acid pump into 1 L bioreactor. Three pH values were evaluated for fed-batch and a simple batch without pH control was done for comparison. The viable cell concentration was compared before and after freeze-drying samples harvested during the cultures. Results: L-glutamic acid was identified as the preferred substrate for rBCG-pertussis. While the fed-batch strategy did not enhance the maximum specific growth rate compared to simple batch cultivation, it did improve the specific growth rate after day 4 in the pH 7.4-controlled fed-batch cultures, thereby reducing the cultivation time. Fed-batch cultures controlled at three pH levels exhibited lower optical density than the simple batch, although the viable cell counts were similar. Notably, samples harvested after day 8 from the simple batch cultures showed a reduction in CFU/mL after freeze-drying, whereas all fed-batch samples exhibited high recovery of viable cell counts post lyophilization. Conclusions: The additional glutamate supplied to the fed-batch cultures may have protected the cells during the lyophilization process.

Physicochemical Characterization of Polysaccharide–Protein Carriers with Immobilized Yeast Cells Obtained Using the Freeze-Drying Technique

New techniques for the immobilization of yeast cells have the potential for enhancement of the beer production process. Alongside conventional materials for cell immobilization, there is a rising trend toward polysaccharide–protein systems. This study focused on the immobilization of yeast cells (Saccharomyces pastorianus) via a freeze-drying process. The whey protein isolate, sodium alginate, maltodextrin, inulin, and their blends were used for carrier preparation. The effect of a 1.0% inulin solution as a cryoprotectant on the viability of the yeast cells after the freeze-drying process was also analyzed. The powders were assessed for cell viability, moisture content, water activity, solubility, particle size, and surface charge. According to the results, the addition of whey proteins reduced the moisture content, while solubility did not significantly decrease. Samples containing whey protein showed slight diameter variations. The negative surface charge observed in all samples, especially the control, indicates a cell’s tendency to aggregate, demonstrated by optical microscopy. SEM micrographs showed successful cell immobilization in polysaccharide–protein carriers. Furthermore, inulin and whey protein addition enhanced cell protection during the immobilization of cells. The freeze-drying technique demonstrates efficacy in immobilization of yeast cells, indicating its potential for applications in the food and beverage industry.

Probiotication of Plum Pulp and Conditions Effects Freeze-Drying in Cell Viability, Functional Properties and Antioxidant Activity

This study investigated the effects of fermenting plum pulp with Bifidobacterium animalis ssp. lactis (BAL) on its physicochemical and bioactive properties, as well as the optimization of the freeze-drying (FD) process to develop a fruit-based probiotic delivery system. Fermentation significantly reduced the pH and total acidity of the pulp, achieving a cell viability of 11 log CFU/mL. The FD process was optimized using a factorial design, with maltodextrin concentration (3, 5, and 7%) and freezing temperature (−150, −100, and −50 °C) as variables. The P2 experiment, which used 7% maltodextrin and freezing at −150 °C, showed the best results in terms of yield (25.67%), cell viability (8 log CFU/g), and probiotic survival rate (97.66%). Samples P5, P6, and P7, prepared with 5% maltodextrin and freezing at −100 °C, exhibited the highest levels of bioactive compounds and antioxidant activity (p < 0.05). During 28 days of storage, all samples maintained cell viability without significant logarithmic reduction. In summary, probiotic plum powders offer an excellent plant-based alternative for probiotic consumption, providing safe levels of beneficial bacteria and bioactive compounds with antioxidant action, meeting health and nutrition needs.

FORMULATION, CHARACTERIZATION AND OPTIMIZATION OF PLGA-CHITOSAN-LOADED FATTY ACID SCAFFOLDS FOR THE TREATMENT OF DIABETIC WOUNDS

Objective: The objective of the current research to formulate Eicosapentanoic Acid/Decosahexanoic Acid (EPA/DHA)incorporated into Chitosan (CS)and Poly-Lactic-Glycolic Acid (PLGA), nanoparticles composite scaffolds to the accelerated diabetic wound healing. The main focus of this present research is to evaluate and develop the chitosan–PLGA biodegradable polymer scaffolds loaded with long-chain omega-3 Polyunsaturated Fatty Acids (PUFA’s) (EPA/DHA). Methods: Nano scaffolds were prepared by solvent evaporation method loaded with CS-PLGA, EPA and DHA to treat diabetic wounds at targeted site as pharmacotherapeutically. Upon investigation, the developed biodegradable crosslinked scaffold possesses matrix degradation, optimal porosity, prolonged drug release action than the non-cross linked scaffold. The prepared formulation containing CS-PLGA loaded with EPA/DHA were formulated as nanoscaffold for wound topical applications was carried out by using freeze drying process. Results: The prepared CS-PLGA nano scaffolds were optimized and evaluated for physicochemical properties, dynamic light scattering with a particle size of 248 nm and zeta of-24mVand Scanning Electron Microscopy (SEM) were found to be spherical. In addition, the optical properties of EPA/DHA and PLGA, along with CS, can be compared by examining their absorption and wavelength (nm) using UV-visible spectroscopy. The structural and functional groups of the prepared end products were characterized by Fourier-Transformed Infrared Spectroscopy (FT-IR) has shown good compatibility with excipients and nanoformulaton, in vitro drug release studies done by using dialysis bag membrane results find that first-order Higuchi model was followed showing 20% release in first 0.2 h. MTT(3-(4,5-dimethylthiazolyl)-2,5-diphenyltetrazolium bromide) assay was carried out and it showed that both crosslinked and non-crosslinked scaffolds(110 and 120%) improved cell growth when compared to control (100%). Conclusion: Finally, the results showed that the PLGA, CS nanoscaffolds containing 98% of PUFA’s (EPA/DHA) have increased in proinflammatory cytokines production at the particular wound site and thus accelerated healing activity, depending on the pre-clinical studies have trespassed, the therapeutic potential to penetrating at wound site. The optimized nanoformulation could be a better formulation for targeting and treatment of diabetic wounds at an optimal ratio.

Optimization of Vacuum Freeze-Drying Process and Quality Evaluation of Stropharia rugosoannulata

Stropharia rugosoannulata is a valuable medicinal and food fungus with high nutritive value. Freeze-drying addresses the storage and transportation challenges of fresh Stropharia rugosoannulata, expanding its market while preserving its flavor and quality more effectively than other drying methods. This study optimizes the vacuum freeze-drying process for Stropharia rugosoannulata using an orthogonal experiment method. The process parameters were optimized to determine their effects on the quality of the vacuum freeze-dried product, including pre-freezing temperature, pre-freezing time, and freeze-drying time. The optimal conditions were identified as a pre-freezing time of 60 h, a pre-freezing temperature of −80 °C, and a freeze-drying time of 72 h. The optimal product exhibited a bright color close to its natural state, with minimal browning and its natural white color maintained post-drying. During the drying process, the internal structure of the raw materials remained intact. After drying, the finished product retained its natural form, making it suitable for sale on the market. The soluble protein content of the vacuum freeze-dried Stropharia rugosoannulata reached 68 mg/g. Optimizing the freeze-drying process can better preserve the tissue structure and bioactive substances of Stropharia rugosoannulata, providing a reference for high-quality food processing and showing potential for sustainable development.

Encapsulation of ɣ-Aminobutyric Acid Compounds Extracted from Germinated Brown Rice by Freeze-Drying Technique

Gamma-aminobutyric acid (GABA) from plants has several bioactivities, such as neurotransmission, anti-cancer cell proliferation, and blood pressure control. Its bioactivities vary when exposed to pH, heat, and ultraviolet. This study analyzed the protective effect of the GABA encapsulation technique using gum arabic (GA) and maltodextrin (MD) and the freeze-drying method. The impact of different ratios of the wall material GA and MD on morphology, GABA content, antioxidant activity, encapsulation efficiency, process yield, and physical properties were analyzed. Results showed that the structure of encapsulated GABA powder was similar to broken glass pieces of various sizes and irregular shapes. The highest GABA content and encapsulation efficiency were, respectively, 90.77 mg/g and 84.36% when using the wall material GA:MD ratio of 2:2. The encapsulated powder’s antioxidant activity was 1.09–1.80 g of encapsulation powder for each formula, which showed no significant difference. GA and MD as the wall material in a 2:2 (w/w) ratio showed the lowest bulk density. The high amount of MD showed the highest Hausner ratio (HR), and Carr’s index (CI) showed high encapsulation efficiency and process yield. The stability of encapsulated GABA powder can be kept in clear glass with a screw cap at 35 °C for 42 days compared to the non-encapsulated one, which can be preserved for only 18 days under the same condition. In conclusion, this study demonstrated that the freeze-drying process for GABA encapsulation preserved GABA component extracts from brown rice while increasing its potential beneficial properties. Using a wall material GA:MD ratio of 2:2 resulted in the maximum GABA content, solubility, and encapsulation efficiency while having the lowest bulk density.

Initial Study of Reduced Graphene Oxide Foams Modified by Mn and Bi as Capacitive Electrode Materials

In a view of application of porous materials in wearable electronics and self-powered systems, reduced graphene oxide (rGO) foams modified by Mn or/and Bi were produced in this study to be used as electrodes for supercapacitors. The hydrothermal method and the freeze-drying processes were used for the preparation of the materials further morphologically, elementally and structurally analyzed. Based on the electrochemical characterization, Bi-modified rGO foam was found to be more a promising material for capacitive electrodes in comparison to the other prepared materials.

Impact of freeze drying on the properties of palmitic acid extracted from Plantain stalk waste

The challenge of effectively preserving and concentrating palmitic acid from plantain stalk waste is compounded by the loss and degradation of the compound during traditional drying and extraction methods, which may lead to reduced yield and altered properties of the extracted palmitic acid. This study was aimed at evaluating the impact of the freeze-drying process on the properties of palmitic acid extracted from plantain stalk waste. The study involved preparing plantain stalks, applying freeze-drying or non-freeze-drying methods, extracting palmitic acid, and characterizing the samples using GC-MS, FTIR, XRD, EDX, and SEM. The GC-MS analysis revealed that freeze-drying significantly increased the concentration of palmitic acid compared to non-freeze-drying, as indicated by the higher peak area and height. FTIR spectra demonstrated that freeze-drying better preserved the structural integrity of palmitic acid, while XRD analysis showed enhanced crystalline structure and increased crystallite size in the freeze-dried sample. Additionally, EDX showed that freeze-drying increased the carbon content and decreased the oxygen content of the material, while SEM analyses indicated that freeze-drying resulted in a more porous and irregular surface compared to the denser, smoother structure of the non-freeze-dried sample. The mass, energy, and cost analysis revealed that freeze-drying resulted in a higher yield of palmitic acid compared to non-freeze-drying methods, which, despite being more cost-effective and requiring less energy, demonstrated a notable trade-off in extraction efficiency. The study showed that freeze-drying significantly improved the preservation, concentration, and structural integrity of palmitic acid extracted from plantain stalk waste compared to the non-freeze-drying method.

Enhancing the volatile organic compound and biomass production by three biocontrol potential bacteria in corn steep liquor growth medium and development of cell freeze-drying process.

This study investigates the traits of three plant growth-promoting (PGP) and antagonistic bacteria, Pseudomonas protegens MP12, Bacillus sp. 3R4, and Bacillus sp. T22, to assess their potential application as biocontrol agents by using the ecofriendly and low-cost substrate Corn Steep Liquor (CSL) medium. Analyses of antagonism through volatile organic compounds (VOCs) production, biofilm formation, and growth performance were carried out. Dual antagonism assay showed that all strains displayed significant antagonistic activity against Botrytis cinerea through VOCs. Gas chromatography demonstrated that strains in the CSL exhibited higher VOCs production than Nutrient medium. Moreover, enhanced biofilm formation analysed by Calgary Biofilm Device, growth and biomass were noted in CSL cultures. Pseudomonas protegens MP12, which showed higher cell concentration and biomass yield, was selected for freeze-drying treatments. Storage cell viability assays evidenced that it can be effectively preserved for nearly 7 months at 4°C. The results here obtained showed that CLS medium enhance VOCs production, biofilm formation, growth and biomass of the antagonistic bacteria of the three strains. Eventually, the more effective strain P. protegens MP12 can be stored for nearly 7 months at 4°C.

Construction and Properties of Ultralow Thermal Conductivity and High Strength Zirconia Aerogel Composites by Freeze-Drying.

Zirconia aerogels possess significant applications, including their use catalyst carriers, thermal insulation materials, and thermal barrier coatings. This is due to their ultrahigh temperature resistance, high porosity, and low thermal conductivity. Nonetheless, the inherent challenges associated with ZrO2 aerogels, such as high brittleness, low compressive strength, and inadequate formability, restrict their potential applications. In this paper, with ultralow thermal conductivity and high strength zirconia aerogel composites with inorganic zirconium salt zirconium carbonate as the raw material, acetic acid as the solvent, polyvinylpyrrolidone (PVP) as the viscosity builder to stabilize the structure of the aerogel during the freeze-drying process. Additionally, yttrium nitrate hexahydrate (Y(NO3)3·6H2O) is employed as a phase stabilizer. The sol-gel method, in conjunction with the freeze-drying process, is utilized to fabricate ZrO2 aerogel composites with an optimized microstructure. The findings indicate that optimal process parameters are achieved with a PVP solution concentration of 2.0 wt % and a zirconium carbonate concentration of 20 wt %. The mechanical properties of the resulting composites reach up to 550 kPa, while the thermal insulation performance exhibits a temperature difference of 207 °C/cm and a thermal conductivity of 0.0504 W/(m·K). This advancement addresses the mechanical stability issues commonly associated with traditional ceramic aerogels and widely used elastic insulating materials, thereby enhancing their applicability as thermal insulation and heat preservation materials.

Effectiveness of Lyoprotectants in Protein Stabilization During Lyophilization.

Background: Proteins are commonly used in the healthcare industry to treat various health conditions, and most proteins are sensitive to physical and chemical changes. Lyophilization, also known as freeze-drying, involves sublimating water in the form of ice from a substance at low pressure, forming a freeze-dried powder that increases its shelf life. Extreme pressure and varying temperatures in the freeze-drying process may damage the protein's structural integrity. Lyoprotectants are commonly used to protect protein conformations. It is important to choose a suitable lyoprotectant to ensure optimal effectiveness. Method: Twenty articles screened from Scopus, Web of Science, and PubMed were included in this review that discussed potential lyoprotectants and their effectiveness with different protein models. Results: Lyoprotectants were categorized into sugars, polyols, surfactants, and amino acids. Lyoprotectants can exhibit significant protective effects towards proteins, either singularly or in combination with another lyoprotectant. They exert various interactions with the protein to stabilize it, such as hydrogen bonding, hydrophobic interactions, electrostatic interactions, and osmoprotection. Conclusions: This review concludes that disaccharides are the most effective lyoprotectants, while other groups of lyoprotectants are best used in combination with other lyoprotectants.

Development of a Single Vial Mass Flow Rate Monitor to Assess Pharmaceutical Freeze Drying Heterogeneity.

During pharmaceutical lyophilization processes, inter-vial drying heterogeneity remains a significant obstacle. Due to differences in heat and mass transfer based on vial position within the freeze drier, edge vials freeze differently, are typically warmer and dry faster than center vials. This vial position-dependent heterogeneity within the freeze dryer leads to tradeoffs during process development. During primary drying, process developers must be careful to avoid shelf temperatures that would result in overheating of edge vials causing the product sublimation interface temperature to rise above the critical (collapse) temperature. However, at lower shelf temperatures, center vials require longer to complete primary drying, risking collapse or melt-back due to incomplete drying. Both situations may result in poor product quality affecting drug stability, activity, and reconstitution times. We present a new approach for monitoring vial location-specific water vapor mass flow based on Tunable Diode Laser Absorption Spectroscopy (TDLAS). The single vial monitor enables measurement of the gas flow velocity, water vapor temperature, and gas concentration from the sublimating ice, enabling the calculation of the mass flow rate which can be used in combination with a heat and mass transfer model to determine vial heat transfer coefficients and product resistance to drying. These parameters can in turn be used for robust and rapid process development and control.

Ultrasound-assisted freeze-drying graphitization process for the fabrication of two-dimensional carbon/Fe3O4 composite aerogels for microwave absorption

Magnetic Fe3O4 materials have received attention from researchers due to their significant wave absorption potential, but there are limitations to their efficient electromagnetic wave absorption and lightweight applications. Combining materials with dielectric properties to optimize the performance of Fe3O4 has become one of the research directions. In particular, carbon nanomaterials, such as graphene, show great application prospects in the field of microwave absorption due to their physical properties. To improve the impedance mismatch issue of graphene, researchers consider combining it with magnetic nanoparticles. Commercial applications require materials that are cost-effective, easy to produce, and environmentally sustainable, driving research on novel 2D carbon materials. In this study, 2D carbon materials were prepared by ultrasound-assisted freeze-drying/graphitization process using polymers as precursors, which simplifies the preparation process and avoids the use of expensive sacrificial templates and catalysts. The 2D carbon materials prepared by this method were used as the dielectric component in the wave-absorbing composites, and the nano effect was utilized to significantly improve the microwave absorption properties of the materials. The maximum reflection loss of the prepared graphite nano-aerogel reaches −84.16 dB and the EAB reaches 3.74 GHz. In addition, by adding Fe3O4 nanoparticles and applying an ultrasonic field for dispersion in the freeze-drying process, the nanoparticle agglomeration is effectively prevented, which provides a simple and efficient pathway for the preparation of nanocomposites.

Microstructure-mechanical property relationships of polymer nanocomposite reinforced with lyophilized montmorillonite/carbon nanotubes hybrid particles

Abstract Introducing multi-walled carbon nanotubes (MWCNT) and montmorillonite (MMT) simultaneously into a polymer can significantly enhance its properties. Meanwhile, choosing the best technique to homogeneously disperse these nanohybrid particles in polymers, without agglomerates, is still a challenge. In this study, a hybrid MMT/MWCNT, prepared by lyophilization process, is introduced in polylactide (PLA). Morphology of the resulting nanocomposites displays synergistic relationships of the MMT/MWCNT, facilitating dispersion in PLA. The analysis of transmission electron microscopy (TEM) specific particle densities of PLA0.5hyb, PLA1.0hyb, and PLA2.0hyb shows values of 77, 64, and 35 µm⁻2, respectively. This suggests that MMT platelets are significantly more exfoliated in PLA0.5hyb compared to the other nanocomposites. It also indicates that filler aggregation increases as the MMT/MWCNT concentration increases. Compared to neat PLA, elastic modulus of nanocomposites increased by up to 46 %, demonstrating the reinforcing effect of MMT/MWCNT hybrid nanofillers. The nanocomposites exhibit viscosity, plasticity and damage phenomena, which are significantly decreased because of the MMT/MWCNT incorporation, compared to neat PLA. Furthermore, the viscoelastic properties, analyzed by dynamic thermal-mechanical analysis, record about 27 % increase in the storage modulus of the nanocomposites compared to PLA, indicating the effectiveness of the hybrid MMT/MWCNT in increasing the resistance of PLA/MMT/MWCNT nanocomposite against thermomechanical aggression.

Freeze-dried wafers containing sesame oil for alleviation of dry mouth

A dry mouth is a condition with significant morbidity. Conventional saliva substitutes are expensive, short-lived, and prone to contamination. This study presents a Freeze-Dried Sesame Oil Emulsion Saliva Substitute (FD-SOESS), which combines the advantages of sesame oil through a freeze-drying process and assesses its effectiveness. High-speed homogenization (HSH) as well as high-pressure homogenization (HPH) techniques were employed to fabricate the FD-SOESS. The formulations that underwent the additional HPH step demonstrated improved physical properties, such as lower viscosity and faster redispersion times, compared to HSH alone. The optimized formulation (F11) possessed a near neutral pH of 6.67 and rapid re-dispersibility that was <141.5 s), which is acceptable for oral administration. Additionally, the FD-SOESS formulation revealed heterogeneous porous structures with a layered arrangement of different pore sizes, and the resulting formulation had low moisture content (2.76 %). The formulation met the microbial limit test. The antioxidant IC₅₀ of sesamin was found to be 0.318 μM. Furthermore, it was not toxic to periodontal cells at 50 μg/mL or 100 μg/mL. Human periodontal cell lines subjected to scratch and treated with FD-SOESS demonstrated notable migration that achieved complete wound closure within two days. The administration of FD-SOESS led to a notable elevation in the mucus concentrations found in the saliva samples of all participants. Overall, the results indicated that FD-SOESS is a highly promising alternative to saliva and may improve oral health for individuals suffering from dry mouth.

Polymeric additives to sustain the dissolution enhancement of niclosamide nanocrystals formed via freeze drying

Nanocrystal formation is an effective method to increase the dissolution of drug compounds with limited solubilities. Niclosamide is a sparingly soluble compound, and it also tends to become an even less soluble monohydrate upon contact with dissolution media. We utilized freeze drying to successfully generate niclosamide nanocrystals, which displayed rapid initial dissolution but also suffered from the expedited formation of the monohydrate. Therefore, we explored some pharmaceutically acceptable polymers to overcome the unfavorable anhydrate-to-monohydrate transformation. Poly(vinylpyrrolidone-co-vinyl acetate) (Mw 45000–70000) effectively retarded the monohydrate formation in a concentration-dependent manner, and 3–5% in the drug-polymer mixture was enough to sustain the enhanced initial dissolution of niclosamide nanocrystals. The area under the dissolution curve tripled due to the combined effect of the nanocrystal formation and the monohydrate inhibition. This study demonstrates an example of the one-pot freeze-drying process to form an optimized drug-additive mixture to realize the full potential of drug nanocrystals.

Novel insight into the cross-linking of typical wheat starch-based food components during freeze-drying: Starch, lipids, proteins and their ternary mixtures

Starch-based foods have a large consumer base worldwide. It is known that the quality of freeze-dried starch-based products is subject to deterioration during the production process. The present study was unprecedented carried out to examine the effects of freeze-drying on the cross-linking between components of gelatinized starch-based system. The results showed that the retrogradation of starch in the process of dehydration, the weakening of the binding capacity between the substrate and water of the freeze-dried product and the weakening of the interaction strength between the components of the product were the key mechanisms leading to the quality deterioration of the wheat starch-based conditioned food during the freeze-drying. The addition of lipid and protein can inhibit starch retrogradation during freeze-drying, and the inhibition effect of oil is better. However, the intervention of oil and fat will cause dehydrated starch to re-adsorb the melted oil/water mixture during the freeze-drying process, resulting in the deterioration of product quality. The intervention of protein will improve the binding ability of freeze-dried wheat starch-based product matrix to water. In the ternary system, the intervention of protein will weaken the inhibition effect of lipid on retrogradation of starch in the freeze-drying process. In addition, the lower drying temperature will lead to the decrease of the interaction strength between the components of ternary mixed system. Avoiding the melting of frozen materials during drying is the key control point to improve the quality of freeze-dried wheat starch-based products.

Ionic liquids-assisted integration of biobased materials for sustainable elaboration of nanocomposites using hydroxyethyl cellulose and interlayered clay for efficient separation of Co(II) from multi-component mixtures

This study focuses on the development of eco-friendly biobased adsorbents through a sustainable hydrothermal and freeze-drying synthesis process, utilizing cost-effective bio-sourced materials to minimize energy consumption and waste. The biobased adsorbents were elaborated using hydroxyethyl cellulose-ionic liquids and bentonite clay. The elaborated biocomposites were characterized using X-ray diffraction (XRD), Fourier-transform infrared spectroscopy/attenuated total reflection (FTIR/ATR), thermogravimetric analysis (TGA), and electron microscopy-energy dispersive X-ray (SEM–EDX), Brunauer–Emmett–Teller (BET) and zeta potential (ZP). Structural analysis confirms the intercalation and incorporation of HEC-ILs polymeric chains into Be-Na matrix and the formation of biocomposites. The [HEC-ILs/Be-Na] composite was subsequently employed for solid-phase extraction of Co(II) by investigating the effect of pH, initial Co(II) concentrations, time, temperature, and the presence of co-existing ions (Na(I), Li(I), Mn(II), Ni(II), and Al(III)). The adsorption kinetics of Co(II) metal ions were suitably characterized using the pseudo-second-order model (with R2 > 0.99). Furthermore, the adsorption isotherms conformed to the Langmuir model (with R2 > 0.97), suggesting a chemisorption process with an adsorption capacity of 69.8 mg/g. The thermodynamic study reveals that the adsorption process exhibits characteristics of spontaneity and endothermicity (ΔH° = 74.197 kJ mol−1, ΔG° < 0 kJ mol−1). The proposed mechanism for Co(II) adsorption on the developed biocomposite involves electrostatic interactions, ion exchange, and anion-π interactions. The biobased composite exhibited remarkable selectivity for Co(II) and demonstrated great potential as an adsorbent for industrial applications.Graphical abstract

Development of Solventless Pharmaceutical Technique for Manufacture of Pharmaceuticals

The aim of our study was to develop a solventless drug pelletization and polymer coating technique for pharmaceutical manufacturing. This review describes a dry coating technique using a mechanical powder processor and a V-shaped blender to produce coated pellets or tablets by mechanically mixing polymer particles and core materials (such as drug pellets and uncoated tablets) without the need for a solvent. First, aqueous latexes comprising colloidal polymethacrylates and ethylcellulose were solidified by freeze drying to produce polymer particles for the dry coating process. These particles and the cores were then subjected to mechanical powder processing or V-shaped blending to provide coated formulations with controlled-release characteristics. Polymer coating was achieved by using agglomerates comprising assembled colloidal polymer. The agglomerated polymer was easily pulverized during the mixing treatments due to its loose structure (the lack of close contacts between the colloidal particles), and the resulting fine polymer with high adhesiveness was deposited on the cores. Colloidal polymer dispersed in aqueous latex tends to coagulate in the freeze-drying process due to condensation of the dispersion, yielding dense agglomerates with poor coating characteristics. The presence of surfactants (such as sodium lauryl sulfate) in the latex can prevent adhesion between colloidal particles in the freeze-drying process, providing loosely structured agglomerates suitable for dry coating. Dry coating with a V-shaped blender could thus be achieved with these polymer particles instead of having to use a mechanical powder processor.