Search Results (1,626)

Background/Objectives: Drug products on the pharmaceutical market must meet a number of requirements that guarantee their quality, safety, and efficacy. Accordingly, periodic inspection of the content of active pharmaceutical ingredients (APIs) in marketed drug products is carried out, confirming that they meet all quality and quantity requirements for a given drug formulation before the expiration date. Therefore, the purpose of this study was to evaluate the suitability of the most commonly used thermal analysis methods, differential thermal analysis (DTA), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA), in the control of the composition of commercially available drug products. Results: Based on a review of the literature, it was shown that thermal methods can be useful in distinguishing drug products from different manufacturers, which guarantees their usefulness in quality control of finished drug products and detecting drug products from illegal manufacturers. They are also useful as tools for confirming the presence of APIs in dosage forms under investigation. The cited literature also indicates that DSC and TGA methods can be used in the quantification of APIs in marketed drug products and to detect non-compliant drug products. The use of chemometric techniques to interpret thermal data can eliminate the adverse effects of excipients on quantification results. Conclusions: Thermal methods are a good complement to chromatographic and spectroscopic methods, with the particular advantages of not needing any sample pretreatment, low sample weight, and short analysis time. Full article

CFRP (carbon fiber-reinforced polymer) production in Europe is approximately 10,000 metric tons annually, and according to the UK authorities, approximately 35% of end-of-life CFRP waste is currently landfilled. The authors propose a novel recycling process for industrial CFRP waste particles to produce the core of a sandwich CFRP panel through the direct molding method. Industrial CFRP powder from grinding operations was collected, sieved and molded into square panels with and without external skins of virgin CFRP prepreg. Thermogravimetric (TGA) and differential scanning calorimetry (DSC) analysis revealed thermal activation (~70 °C), indicating potential for reprocessing. This study proposes a novel recycling route that directly molds industrial CFRP grinding waste into the core of sandwich structures, with or without virgin CFRP prepreg skins. Key findings: thermal re-processability was confirmed through TGA and DSC, showing activation near 70 °C; electrical conductivity reached 0.045 S/cm through the thickness in sandwich panels, with recycled cores maintaining comparable conductivity (0.04 S/cm); mechanical performance was improved significantly with prepreg skins, as evidenced by three-point bending tests showing enhanced stiffness and strength. These results demonstrate the potential of recycled CFRP waste in multifunctional structural applications, supporting circular economy goals in composite materials engineering. Full article

Enhancing protein–protein interactions is a key therapeutic strategy to ensure effective protein function in terms of pharmacokinetics and pharmacodynamics and can be accomplished with methods like directed evolution or rationale design. Previously, two papers suggested the possible enhancement of protein–protein binding affinity via destabilizing mutations. This paper reviews the results of the previous literature and adds new data to show the generality of the strategy that destabilizing the unbound protein without significantly changing the free energy of the complex can enhance protein–protein interactions for therapeutic benefit. The first example presented is that of a variant of human growth hormone (hGHv) containing 15 mutations that improve the binding to the hGH binding protein (hGHbp) by 400-fold while retaining full biological activity. The second example is that of the YTE mutations (M252Y/S354T/T256E) in the Fc region of a monoclonal antibody (mAb). The YTE mutations improve the binding of the mAb to FcRn at pH 6.0 10-fold, resulting in elongated serum half-life of the mAb. In both cases, (i) chemical titration or differential scanning calorimetry (DSC) showed the mutations destabilize the unbound mutant proteins, (ii) isothermal titration calorimetry (ITC) showed extremely favorable enthalpy (ΔH) and unfavorable entropy (ΔS) upon binding to their respective target molecule compared with the wildtype, and (iii) hydrogen/deuterium exchange–mass spectrometry (HDX-MS) revealed that these mutations increase the free energy of unbound mutant protein without significantly affecting the free energy of the bound state, resulting in an enhancement to the binding affinities. The third example presented is that of the JAWA mutations (T437R/K248E) also located in the Fc region of a mAb. The JAWA mutations facilitate antibody multimerization upon binding to cell surface antigens, allowing for enhanced agonism and effector functions. Both DSC and HDX-MS showed that the JAWA mutations destabilize the unbound Fc, although the complex was not characterized due to weak binding. Enhancement of protein–protein interactions through incorporation of mutations that increase the free energy of a protein’s unbound state represents an alternative route to decreasing the protein–protein complex free energy through optimization of the binding interface. Full article

Ready-to-eat products are very popular and controversial due to their microbial safety. The main processing steps in obtaining a safe, edible product is heat treatment. The traditional manufacturing of meatballs, which conducts unhealthy compounds related to deep-fat-fried foods like the oil oxidation of harmful substances and polycyclic aromatic hydrocarbons, has been replaced with baking (180 °C) and steaming (94 °C). The addition of aqueous extract from two herbs, lemon balm (Melissa officinalis L.) or wild thyme (Thymus serpyllum L.), has led to twelve variants of meatballs, obtained from the tenderloin of three different animal species (pork, turkey, and beef). During processing, the food components go through conformational changes that affect the texture of the final product. In this study, differential scanning calorimetry for detecting and characterizing the thermal changes in meatballs was used. In addition, the influence of heat treatments on the textural and rheological parameters of meatballs was evaluated using instrumental methods. The cooking yield registered values of 61.21 ± 0.25% for steamed beef samples and 81.36 ± 0.86% for steamed turkey samples. The latest samples also showed the lowest firmness value, 3.41 ± 0.79 N. In this study, the addition of aqueous extracts did not considerably affect the texture and rheological behavior, which were influenced mainly by the heat treatment and meat type. Generally, steaming determined a firmer texture compared to baking. Full article

Poly(L-lactic acid) (PLLA) and iron (Fe) are popular bioresorbable material candidates for biomedical implants. However, PLLA coronary stents are relatively too thick compared to metallic stents when providing the same mechanical strength, while iron degrades too slowly. Recent studies show that PLLA coatings can enhance iron’s corrosion rate, and iron has strong mechanical strength, making PLLA–Fe composites ideal for bioresorbable implants. Although PLLA coatings on iron samples have been studied, research on embedding iron wires in relatively thick PLLA matrices is limited. Moreover, no studies have yet explored 3D-printed metal wire-reinforced PLLA monofilaments for biomedical applications. To address these research gaps and investigate the in vitro degradation profile of PLLA/Fe wire monofilaments for bioresorbable stents, this study first developed a novel polymer filament–metal wire coextrusion 3D printer for printing PLLA/Fe wire monofilaments. In vitro degradation tests were then conducted on both PLLA/Fe and neat PLLA monofilaments at 50 °C. Thereafter, characterizations, including mass loss, pH, surface appearance and morphology, tensile tests, gel permeation chromatography (GPC), and differential scanning calorimetry (DSC), were performed. Results indicated that the overall degradation rate of PLLA/Fe monofilaments was higher than that of PLLA counterparts, while the degradation rate of PLLA matrix was not affected by the embedded iron wire according to molecular weight analysis. Notably, the Young’s modulus and stiffness of PLLA monofilaments were significantly improved by the iron wires during the early stages of degradation, but the reinforcement in tensile strength was negative after immersion due to the poor embedding quality of the iron wires in the PLLA monofilaments. With future improvement of the embedding quality of iron wire, the 3D-printed PLLA/Fe wire composites can have great potential in the development of biomedical devices using the novel 3D printing method, including most types of stents and bone scaffolds. Full article

In this study, supramolecular inclusion complexes composed of komecosanol (Ko), a lipophilic compound derived from rice bran, and α-cyclodextrin (αCD) were prepared using a solvent-free three-dimensional (3D) ball milling method. Their physicochemical properties were examined using various techniques. Powder X-ray diffraction analysis of the ground mixture at a Ko/αCD ratio of 1/8 revealed the disappearance of diffraction peaks characteristic of Ko and the emergence of new peaks, indicating the formation of a distinct crystalline phase. Moreover, differential scanning calorimetry analysis showed the disappearance of the endothermic peaks corresponding to Ko, indicating molecular-level interactions with αCD. Near-infrared spectroscopy results suggested the formation of hydrogen bonds between the C–H groups of Ko and the O–H groups of αCD. Solid-state ¹³C CP/MAS NMR and T₁ relaxation time measurements indicated the formation of a pseudopolyrotaxane structure, while scanning electron microscopy images confirmed distinct morphological changes consistent with complex formation. These findings demonstrate that 3D ball milling facilitates the formation of Ko/αCD inclusion complexes with a supramolecular architecture, providing a novel approach to improve the formulation and bioavailability of poorly water-soluble lipophilic compounds. Full article

Background: Silkworm cocoons are rich in bioactive compounds beneficial for cosmetic applications. This study presented a novel approach by comparing microwave and ultrasonic pretreatments to enhance silk protein extraction efficiency. The aim was to evaluate the effects of pretreatment methods and extraction solvents on the bioactive components, physicochemical properties, and biological activities of silkworm cocoon extracts for cosmetic applications. Methods: Cocoons of Bombyx mori (Nang Lai) were pretreated using conventional soaking (12 h), microwave (3 min), or ultrasonication (30 min), and then subjected to aqueous or enzymatic extraction. The extracts were analyzed for protein, phenolic, and flavonoid content. Structural and thermal properties were characterized using infrared spectroscopy, X-ray diffraction, differential scanning calorimetry, and thermogravimetric analysis. Antioxidant and anti-aging properties were assessed by measuring the inhibition of nitric oxide, 2,2-diphenyl-1-picrylhydrazyl (DPPH^•), and collagenase. Skin moisturizing effects and irritation potential were tested. Results: Silkworm cocoons pretreated with microwave (ALM) and ultrasonication (ALS), followed by enzymatic extraction, had the highest yields (21.6 ± 0.5% and 21.7 ± 0.4%, respectively). Despite their slightly lower protein contents, these extracts showed elevated phenolic and flavonoid content. ALM and ALS demonstrated strong antioxidant activities, with DPPH^• scavenging of 65.9 ± 0.2% and 65.2 ± 0.3%, collagenase inhibition of 60.3 ± 0.8% and 59.7 ± 1.7%, and nitric oxide inhibition of 13.5 ± 0.4% and 12.9 ± 0.2%, respectively. Skin moisturizing effects increased by 63.6 ± 2.1% for ALM and 61.2 ± 1.5% for ALS, compared to 1.3 ± 0.6% in the control. All extracts were found to be non-irritating for topical application, indicating their safety for skincare formulations. Conclusions: Microwave and ultrasonication pretreatments, in combination with enzymatic extraction, provide an effective, time-efficient, and sustainable method for producing silkworm cocoon extracts with promising cosmetic applications. Full article

Constitutive models and deformation behaviors for polymer materials have long been complex and are always a hot research focus. As a typical semi-crystalline polymer, polyethylene (PE) gas pipes exhibit pronounced nonlinearity, strain dependence, and time dependence during long-term service. Simple material models fail to capture the scale-dependent characteristics of the PE pipes, resulting in difficulties in accurately describing and simulating their deformation and damage behavior. Currently, some PE gas pipes have entered the mid-to-late stages of service life, so it is necessary to propose a constitutive model representing their complex mechanical behavior for simulation and performance evaluation purposes. Based on results from aging tests, tensile tests, differential scanning calorimetry, and Fourier-transform infrared spectroscopy, this study proposes a method to select a rheological framework and a constitutive model that couples thermo-oxidative aging effects in PE gas pipes. The model is developed within the widely recognized rheological framework and is grounded in continuum mechanics, continuum damage mechanics, and the aging behavior of polymer materials. This method and model are suitable for characterizing the mechanical dependency of PE pipes and demonstrate strong fitting performance. According to the calculation results, the goodness of fit of this constitutive model for the uniaxial tensile test results at the different aging times ranges from 0.982 to 0.999. The findings provide theoretical support for the simulation and service life prediction for PE pipelines. Full article

Carbon fiber-reinforced polymer (CFRP) composites are widely used in aerospace due to their excellent strength-to-weight ratio and tailorable properties. However, these properties critically depend on the CFRP curing cycle. The commonly adopted manufacturer-recommended curing cycle (MRCC), designed to accommodate the most conservative conditions, involves prolonged curing times and high energy consumption. To overcome these limitations, this study proposes an efficient and adaptable method to determine the optimal curing cycle. The effects of varying heating rates on resin dynamic and isothermal–exothermic behavior were characterized via reaction kinetics analysis using differential scanning calorimetry (DSC) and rheological measurements. The activation energy of the reaction system was substituted into the modified Sun–Gang model, and the parameters were estimated using a particle swarm optimization algorithm. Based on the curing kinetic behavior of the resin, CFRP compression molding process orthogonal experiments were conducted. A weighted scoring system incorporating strength, energy consumption, and cycle time enabled multidimensional evaluation of optimized solutions. Applying this curing cycle optimization method to a commercial epoxy resin increased efficiency by 247.22% and reduced energy consumption by 35.7% while meeting general product performance requirements. These results confirm the method’s reliability and its significance for improving production efficiency. Full article

Background: Attachments are essential components in clear aligner therapy, enhancing retention and improving the predictability of tooth movements. Mechanical and wear properties of the composite resins used for attachment reproduction are critical to maintaining their integrity and shape over time. This study aimed to evaluate and compare the mechanical properties, thermal behavior, and wear performance of the hybrid composite Aligner Connect (AC) and the flowable resin (Connect Flow, CF). Methods: Twenty samples (ten AC and ten CF) were reproduced. All specimens underwent differential scanning calorimetry (DSC), combustion analysis, flat instrumented indentation, compression stress relaxation tests, and tribological analysis. A 3D wear profile reconstruction was performed to assess wear surfaces. Results: DSC and combustion analyses revealed distinct thermal transitions, with CF showing significantly lower Tg values (103.8 °C/81.4 °C) than AC (110.8 °C/89.6 °C) and lower residual mass after combustion (23% vs. 61%), reflecting reduced filler content and greater polymer mobility. AC exhibited superior mechanical properties, with higher maximum load (585.9 ± 22.36 N) and elastic modulus (231.5 ± 9.1 MPa) than CF (290.2 ± 5.52 N; 156 ± 10.5 MPa). Stress relaxation decrease was less pronounced in AC (18 ± 4%) than in CF (20 ± 4%). AC also showed a significantly higher friction coefficient (0.62 ± 0.060) than CF (0.55 ± 0.095), along with greater wear volume (0.012 ± 0.0055 mm³ vs. 0.0070 ± 0.0083 mm³) and maximum depth (36.88 ± 3.642 µm vs. 17.91 ± 3.387 µm). Surface roughness before wear was higher for AC (Ra, 0.577 ± 0.035 µm; Rt, 4.369 ± 0.521 µm) than for CF (Ra, 0.337 ± 0.070 µm; Rt, 2.862 ± 0.549 µm). After wear tests, roughness values converged (Ra, 0.247 ± 0.036 µm for AC; Ra, 0.236 ± 0.019 µm for CF) indicating smoothened and similar surfaces for both composites. Conclusions: The hybrid nanocomposite demonstrated greater properties in terms of stiffness, load-bearing capacity, and structural integrity when compared with flowable resin. Its use may ensure more durable attachment integrity and improved aligner–tooth interface performance over time. Full article

Ceramic pastes used in additive manufacturing offer several advantages, including low production costs due to the availability of raw materials and efficient processing methods, as well as a reduced environmental footprint through minimized material waste, optimized resource use, and the inclusion of recyclable or sustainably sourced components. This study evaluates the effect of diatomite content in a ceramic paste composed of carboxymethyl cellulose, kaolinite, and feldspar on its extrusion behavior and thermal conductivity, with additional analysis of its implications for microstructure, mechanical properties, and thermal performance. Four ceramic pastes were prepared with diatomite additions of 0, 10, 30, and 60% by weight. Thermal conductivity, extrusion behavior, morphology, and distribution were examined using scanning electron microscopy (SEM), while thermal degradation was assessed through thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The results show that increasing diatomite content leads to a reduction in thermal conductivity, which ranged from 0.719 W/(m·°C) for the control sample to 0.515 W/(m·°C) for the 60% diatomite sample, as well as an improvement in extrusion behavior. The ceramic paste demonstrated adequate extrusion performance for 3D printing at diatomite contents above 30%. These findings lay the groundwork for future research and optimization in the development of functional ceramic pastes for advanced manufacturing applications. Full article

Ozone is a powerful destructive agent in the oxidative process of polymer composites. The destructive ability of ozone depends primarily on its concentration, duration of exposure, the type of polymer, and its matrix structure. In this work, nonwoven PLA/NR fibers with natural rubber contents of 5, 10, and 15 wt.% were obtained, which were then subjected to ozone oxidation for 800 min. The effect of ozone treatment was estimated using various methods of physicochemical analysis. The visual effect was manifested in the form of a change in the color of PLA/NR fibers. The method of differential scanning calorimetry revealed a change in the thermophysical characteristics. The glass transition and cold crystallization temperatures of polylactide shifted toward lower temperatures, and the degree of crystallinity increased. It was found that in PLA/NR fiber samples, the degradation process predominates over the crosslinking process, as an increase in the melt flow rate by 1.5–1.6 times and a decrease in the correlation time determined by the electron paramagnetic resonance method were observed. The IR Fourier method recorded a change in the chemical structure during ozone oxidation. The intensity of the ether bond bands changed, and new bands appeared at 1640 and 1537 cm⁻¹, which corresponded to the formation of –C=C– bonds. Full article

In this work, we report a novel mechanochemical synthesis method for the synthesis of quinoxaline derivatives—a spiral gas–solid two-phase flow approach, which enables the efficient preparation of quinoxaline compounds. Compared to conventional synthetic methods, this approach eliminates the need for heating or solvents while significantly reducing reaction time. The structures of the synthesized compounds were characterized using nuclear magnetic resonance (NMR), Fourier-transform infrared spectroscopy (FT-IR), ultraviolet-visible (UV–Vis) absorption spectroscopy, powder X-ray diffraction (XRD), differential scanning calorimetry (DSC), and high-performance liquid chromatography (HPLC). Using the synthesis of 2,3-diphenylquinoxaline (1) as a model reaction, the synthetic process was investigated with UV–Vis spectroscopy. The results demonstrate that when the total feed amount was 2 g with a carrier gas pressure of 0.8 MPa, the reaction completed within 2 min, achieving a yield of 93%. Furthermore, kinetic analysis of the reaction mechanism was performed by monitoring the UV–Vis spectra of the products at different time intervals. The results indicate that the synthesis of 1 follows the A4 kinetic model, which describes a two-dimensional diffusion-controlled product growth process following decelerated nucleation. Full article

Background/Objectives: Parenteral nutrition (PN) supports patients unable to receive nutrients via the gastrointestinal tract, but it lacks the health-promoting natural bioactive compounds found in a typical oral diet. This study aimed to develop a human serum albumin-based intravenous delivery system for lutein (an antioxidant carotenoid with vision-supportive and hepatoprotective properties) as a PN additive. Methods: An albumin–lutein nanosuspension (AlbLuteN) was synthesized using a modified nanoparticle albumin-bound (nab^TM) technology and characterized physicochemically. The nanoformulation was added to four commercial PN admixtures to assess the supplementation safety throughout the maximum infusion period. Visual inspection and measurements of fat globules larger than 5 µm (PFAT5) and the mean hydrodynamic diameter (Z-average), zeta potential, pH, osmolality, and lutein content were performed to detect potential interactions and evaluate the physicochemical stability. Results: AlbLuteN consisted of uniform particles (Z-average of 133.5 ± 2.8 nm) with a zeta potential of −28.1 ± 1.8 mV, lutein content of 4.76 ± 0.39%, and entrapment efficiency of 84.4 ± 6.3%. Differential scanning calorimetry confirmed the amorphous state of lutein in the nanosuspension. AlbLuteN was successfully incorporated into PN admixtures, without visible phase separation or significant changes in physicochemical parameters. The PFAT5 and Z-average values remained within pharmacopeial limits over 24 h. No substantial shifts in zeta potential, pH, or osmolality were observed. The lutein content remained stable, with losses below 3%. Conclusions: AlbLuteN can be safely added to representative PN admixtures without compromising their stability. This approach offers a novel strategy for intravenous lutein delivery and may contribute to improving the nutritional profile of PN. Full article

We present an alternative to the classical SQUID magnetometric measurements for the First-Order Reversal Curve (FORC) diagram approach by employing differential scanning calorimetry (DSC) experiments. After discussing the main results, the advantages and limitations of the magnetometric FORCs, we introduce the calorimetric method. We argue that, while the results are comparable to those obtained via magnetometry, the calorimetric method not only significantly simplifies the required mathematical computations but also detects subtle or overlapping phase transitions that might be hard to distinguish magnetically. The methodology is illustrated through both experimental data and mean-field simulations. Full article