Hydrolysis Products Research Articles

Biochemical Characterization of Mannanase from Newly Isolated Acinetobacter sp. KUB-ST1-1 and its Hydrolysate Containing Mannooligosaccharides: Potential as Applied Prebiotic for Pet Food

The β-mannanase enzyme derived from isolated Acinetobacter sp. KUB-ST1-1 was studied for its potential for mannooligosaccharide production. Extracellular mannanase from Acinetobacter sp. KUB-ST1-1, cultured in nutrient broth with 0.5% (w/v) locust bean gum, was purified using ultrafiltration, anion exchange chromatography, and cation exchange chromatography. The enzyme, with a molecular weight of 57 kDa, had high activity in a 50 mM phosphate buffer at pH 6.0 and was stable from pH 4.0 to 7.0. It had high-temperature stability at 40 °C and 50 °C for up to 18 h. This enzyme was highly active toward konjac and galactomannan, especially with locust bean gum and copra meal. The hydrolysis products consisted mainly of the 2 and 3 units of mannooligosaccharide. The mannooligosaccharide exhibited prebiotic properties by promoting increased growth of some beneficial lactic acid bacteria. Furthermore, the defatted copra meal hydrolysate had considerable resistance to pepsin, trypsin, and bile salts under simulated gastrointestinal conditions for dogs. These characteristics highlighted the enzyme's excellent properties and suggested its potential as a promising candidate for applications in the food and bio-industries, particularly in pet food production.

Structural evolution of iron components and their action behavior on lignite combustion

Spontaneous combustion of lignite is closely related to the inherent minerals it contains, and the iron component has a remarkable influence on the combustion property of lignite. It is very important to study the influence of iron component on the combustion reaction property of lignite to reveal autoignition mechanism of lignite and reduce autoignition of lignite. In this research, FeCl3 and Fe2O3 were doped into demineralised lignite (SL+) by impregnation to research the effects of iron salts and iron oxides on the combustion properties of lignite. Based on the above, the effects of post-treatment method of the FeCl3-doped coal samples, iron-salt hydrolysis products and heat-treated temperatures on the combustion property of lignite were researched, and the microstructures of the coal samples were characterised and analysed using Fourier transform infrared spectroscopy (FTIR), Scanning electron microscope-energy dispersive spectrometer (SEM-EDS), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The results demonstrate that doping with FeCl3 increases the combustion performance of lignite, thereby reducing the ignition temperature of lignite by approximately 112 °C. In contrast, doping with Fe2O3 has a weaker combustion-promoting effect. XRD and XPS characterisation indicates that iron species in the coal samples doped with iron salts are highly dispersed and exhibit the FeOOH structure, whereas iron species in the coal samples doped with Fe2O3 exhibit the crystal form of α-Fe2O3. Doping of lignite with FeCl3 and its hydrolysis product β-FeOOH reduces the ignition temperature of the coal samples. Iron species in the FeCl3-doped coal samples after heat treatment at 300 °C-500 °C increase the combustion property of the coal samples, whereas iron species after heat treatment at 600 °C-900 °C have a much weaker or non-existent promoting effect on the combustion performance of the coal samples. The characterisation show a change in iron species in the coal samples with the rise in the heat treatment temperature. This change progresses from highly dispersed β-FeOOH below 300 °C to Fe3O4 above 400 °C. Fe3O4 is gradually reduced, with part of it further reduced to elementary iron at the same time as grain growth. It is believed that the gradual agglomeration of Fe3O4 and the appearance of elementary iron are the main reasons for the weakening or disappearance of the promoting effect on coal combustion.

Pulsed Electric Field Pretreatment Enhances the Enzyme Hydrolysis of Baker’s Yeast

Baker’s yeast is a key starting material for producing extracts with diverse compositions and applications. This study investigates the effect of pulsed electric field (PEF) pretreatment, which induces irreversible electropermeabilization, on the enzymatic hydrolysis of yeast. Cell suspensions were exposed to monopolar rectangular pulses in a continuous flow system followed by 4 h of incubation with Alcalase at concentrations of 0.2% and 0.5%. PEF pretreatment significantly improved enzymatic hydrolysis, with maximum intracellular content recovery under electrical conditions resulting in outlet temperatures of 56–58 °C. The released protein reached 163.7 ± 13 mg per gram of dry cell weight (DCW). SDS-PAGE analysis showed that the extracts predominantly contained peptides with molecular masses below 4.7 kDa. The phenolic content was comparable to that of cell lysates obtained after mechanical disruption. The free α-amino nitrogen content and total antioxidant activity reached 218.2 ± 26 mg/gDCW and 53.4 ± 4.6 mg TE/gDCW, respectively, representing 3.2-fold and 2.65-fold increases compared to cell lysates. The hydrolysates from PEF-pretreated cells demonstrated a positive effect on the proliferation of the human keratinocyte cell line HaCat. The obtained data lead to the conclusion that PEF pretreatment is a promising approach to enhance the production of yeast hydrolysates with various applications.

Hydrolytic instability of laser-ablatively deposited CaSi2 coatings in air and neutral water affects the behavior of bone healing-related cell types

Calcium silicide (CaSi2) instability in humid air or pH-neutral water remains unknown, although the topochemical formation of silicene from CaSi2 in various aqueous phases is a well-known process. Here we report on laser ablation of CaSi2 in the vacuum and ethanol, characterize coatings deposited on titanium substrates with electron microscopy, X-ray photoelectron, Raman, and infrared spectroscopy, and examine the instability of the deposited coatings in humid air and neutral water. We further investigate the behavior of human mesenchymal stromal cells (hMSCs), vascular cells (HUVECS, human umbilical vein endothelial cells), and macrophages (derived from THP-1 cell line) in contact with the deposited coatings submerged in cell culture medium. The observed results indicate that the CaSi2 coatings undergo topochemical conversion to silicene, which is accompanied by hydrolytic reactions leading to inorganic Ca compounds and SiO2, and that the response of all cell types in the hydrolyzed CaSi2 surface domain is negatively affected by the nature of the hydrolytic products. In contrast, cells showed a tendency for enhanced biocompatibility towards the CaSi2 particles ablated in the vacuum. The results suggest that coating approaches can significantly influence cell behavior outcomes.

Preparation of wheat germ albumin polypeptide microcapsules embedded with starch sodium octenylsuccinate/sodium alginate-based materials and sustained-release properties in vitro

The enzymatic hydrolysis products of wheat germ albumin have been extensively studied due to their strong antioxidant properties. The small intestine is an important part for absorbing active substances, but polypeptides are not acid-resistant and are easily hydrolyzed and lose their activity in the stomach, which does not achieve the effect of small intestine absorption. In this study, the optimal process conditions for microencapsulation of wheat germ albumin polypeptides were determined based on response surface optimization experiments as follows: wall to material ratio (starch sodium octenylsuccinate (SSOS) : sodium alginate (SA) =3:1), homogenization time 10 min, and wall to core ratio 20:1. The embedding rate of microcapsules prepared under these conditions was 65.33%. The average particle size of microcapsules was 100.21 μm. SEM results showed that the freeze-drying microcapsules had a sheet-like structure. The increased intensity of the amide A band in the microcapsules in Fourier transform infrared (FT-IR) spectroscopy indicated the formation of hydrogen bonds between the wall materials, while thermogravimetric analysis confirmed the protective effect of microcapsules on the formation of wheat germ albumin polypeptides. The release rates of microcapsules in gastric and intestinal juice were 26.54% and 84.41%, respectively, indicating that microcapsules had a sustained release effect.

A simplified ratiometric fluorescent sensing strategy for enhanced detection of alkaline phosphatase employing Prussian blue nanozymes and commercially available chromogen

The traditional nanozymes-based ratiometric fluorescence sensing platforms usually necessitate the supplementary addition of fluorescent probes, therefore greatly restricting its convenient and broad application. In this study, a highly sensitive and selective ratiometric fluorescence platform for alkaline phosphatase (ALP) detection was established, only employing Prussian blue (PB) nanozymes and a commercially available chromogen of o-phenylenediamine (OPD). PB nanozymes with remarkable peroxidase-like (POD-like) activity can effectively catalyze OPD chromogen to yield 2,3-diaminophenazine (OPDox) with an intense yellow fluorescence at 573 nm emission peak. Target ALP can facilitate ascorbic acid 2-phosphate (AAP) dephosphorylation to generate phosphate and ascorbic acid (AA). Significantly, both these two resultant hydrolysis products could effectively decrease the OPDox generation via a dual-path based inhibition on the PB nanozymes POD-like activity. On the other hand, the generated dehydroascorbic acid (DHAA) from AA oxidation would exclusively react with OPD chromogen to yield 3-(dihydroxyethyl)furo[3,4-b]quinoxaline-1-one (DFQ) with a strong blue fluorescent signal at 434 nm, which further providing a significant enhancement on the sensing selectivity of ALP detection. As a result, an increased yellow fluorescence of OPDox and decreased blue fluorescence of DFQ could be clearly observed with different ALP addition. A robust linear relationship between the fluorescence ratio of F434/F573 and ALP activity ranging from 0.25 U/L to 6 U/L was obtained, with a low detection limit of 0.112 U/L. This proposed method demonstrates high sensitivity, excellent selectivity, cost-effectiveness, and operational simplicity, yet enabling an effective detection of ALP levels in human serum.

Hydrolysis rate and mechanism of water-dispersed polyesters with different sulfonate group contents in the cutinase-catalyzed system.

Water-dispersed polyester (WPET) has irreplaceable and wide application prospects in the textile field, but it is easy to form printing and dyeing wastewater during traditional fabric treatment. In this paper, cutinase-catalyzed green hydrolysis of WPET was achieved. The main purpose of this paper is to study the difference between two PEG-free WPETs with different -SO3- content in the cutinase-catalyzed hydrolysis process. Differences in solution properties, enzyme activity, SSIPA, and TPA release as well as functional groups and thermal properties of the hydrolysis products of the systems during cutinase hydrolysis were analyzed in detail for 14.1 % S-0 % PEG and 9.5 % S-0 % PEG. Results show that the structure of WPET has an influential effect on its hydrolysis rate in cutinase-catalyzed systems, which mainly originates from the -SO3- content. SSIPA released by WPET during hydrolysis has an inhibitory effect on cutinase enzyme activity. The hydrolysis process of WPET with higher -SO3- content releases more SSIPA, which in turn inhibits the enzyme activity of cutinase in the reaction system, ultimately leading to a slower hydrolysis rate of WPET. These findings provide new ideas for cutinase to target WPETs with different structures and are important for the green development of the textile industry.

A high-performance flame retardant liquid synthesized on the basis of DOPO hydrolysis products avoids the defects of DOPO

It was first proposed to use 2-(2-hydroxyphenyl) phenyl phosphonic acid (HPPA), which is hydrolysis product of DOPO, has a structure more similar to EP, to replace DOPO in the preparation of flame retardant, and finally synthesized a highly efficient liquid flame retardant DP based on HPPA, the theoretical phosphorus content of DP is up to 17.5wt%, so EP can achieve excellent flame retardant/inhibit combustion effect with a small amount addition of DP. For example, the LOI of EP/DP6.0 is increased to 41.2 % and reaches the V-0 rate of UL-94, the PHRR and THR are reduced by 52.4 % and 45.2 % respectively, in addition, the addition of DP in small quantities does not destroy the overall performance of EP, maintains and improves the excellent mechanical and thermal properties of epoxy resin as a whole, and DP has excellent curing promoting effects, meeting the processing and use requirement of high performance EP. It is better than DOPO overall and has good application prospects.

Enhanced physicochemical characteristics and biological activities of low-temperature ethylenediamine/urea pretreated lignin.

Low-temperature ethylenediamine (EDA)/urea pretreatment had been demonstrated to be an efficient pretreatment method for enzymatic hydrolysis and bioethanol production. For high-value utilization of the third main components of lignocellulosic biomass, the physicochemical structure characteristics and biological activities of low-temperature EDA/urea pretreated lignin (EUL) were comprehensively investigated in the present study. The results demonstrated that the pretreatment process facilitated the depolymerization of lignin, resulting in notable reduction in molecular weight and polydispersity index from 2.32 to 1.42kg/mol and 1.44 to 1.20, respectively. The EDA/urea pretreated lignin (EUL) exhibited enhanced ultraviolet absorption capacity and the most significant DPPH radical scavenging and inhibition of Staphylococcus aureus in comparison to the primary lignin (PL) and the NaOH pretreated lignin (NL). Enhanced physicochemical characteristics and biological activities of EUL make it more suitable to be developed as sunscreen ingredient or antioxidant and antimicrobial agent in food preservation and conservation.

Macro-Superlubricity Induced by Tribocatalysis of High-Entropy Ceramics.

Macroscale superlubricity has attracted considerable attention as a promising strategy to minimize frictional energy dissipation and achieve near-zero wear. However, realizing macroscale superlubricity with prolonged durability remains an immense challenge, particularly on engineering steels. Current superlubricants render steel surfaces susceptible to corrosion, causing severe wear and superlubrication failure. Herein, high-entropy ceramics (HEC) with catalytic properties are innovatively introduced to prevent corrosion of engineering steels and achieve macro-superlubricity through tribo-catalytic effect. Furthermore, this catalytically induced superlubricity system exhibits an ultra-low friction coefficient of 0.0037 under contact pressure up to 1.47 GPa, an ultra-long cycle lifetime of 1.25 × 106 cycles (corresponding sliding distance up to 5 km), and an extremely low wear rate of 3.032 × 10-10 mm3·N-1·m-1 on the HEC surface. Based on the experimental analysis and theoretical simulation, the in situ formed HEC nanocrystals reduce the Gibbs free energy of hydrolysis of PA molecules into inositol and phosphoric acid molecules in the lubricant. Notably, the hydrolysis products favorably contributed to the reduction of shear force in the lubrication system, which is essential for achieving macroscale superlubricity over a long time. This study provides a new perspective for designing robust superlubricity systems by harnessing the tribocatalytic effect of high-entropy materials.

Antihypertensive, Anti-Inflammatory, and Antiangiogenic In Silico Activity of Lactoferrin-Derived Peptides of Equine Milk Hydrolysate

Background: Equine milk, including its whey proteins, is a source of nutrients and functional components in the human diet, and is especially beneficial for people with weakened immune systems, newborns, and athletes. Objectives Whey proteins in equine milk constitute approximately 20% of the total protein content and include various fractions such as albumin, globulin, and lactoferrin. Lactoferrin is one of the most extensively studied whey proteins in equine milk. Methods: HPLC-Mass analysis, enzymatic hydrolysis, modeling of 3D structure and biological activity in silico. Results:It has antioxidant, anti-inflammatory, and immunomodulatory properties, making it a promising candidate for influencing the various aspects of cardiovascular disease pathogenesis. The products of Lactoferrin hydrolysis by trypsin were confirmed using HPLC. The half-lives of the hydrolysate in the bloodstream and in an intestine-like environment were predicted in silico. Various biological activities (antihypertensive, anti-inflammatory, and antiangiogenic) were also estimated in silico and compared with the corresponding activities of lactoferrin hydrolysate amino acid sequences from camel and dromedary milk. Conclusions:The three-dimensional modeling of lactoferrin hydrolysate peptides was performed to support the development of computational models or simulations, as well as to investigate their potential antimicrobial, anti-inflammatory, or immune-modulating functions in clinical or nutritional applications.

A Novel Thermostable Laminarinase with High Activity from Streptomyces albus and Its Catalytic Characteristics in Laminarin Degradation.

Laminarin oligosaccharides (LOSs) degraded from laminarin present nutritional functions. Laminarinases with high activity and good stability are significant tools for LOS production. OUC-SaLam66, a novel GH128 laminarinase from Streptomyces albus, was heterologously expressed. OUC-SaLam66 harbored a significant activity advantage up to 2294.80 U/mg at 45 °C and pH 4.0; meanwhile, it could preserve 80% activity at 45 °C for 12 h, indicating good stability. Significantly, its residual activity was over 75% after incubating at 100 °C for 1 h. Differential scanning calorimetry and molecular dynamic modeling revealed that its melting point and RMSD average point were 114.83 °C and 0.125 nm at 100 °C, respectively, which further proved its superior stability. Its apparent Km and Vmax against laminarin were 6.437 mM and 2.5 μg/min/mg, respectively. Hydrolysis products were mainly composed of laminaritriose and laminaribiose. The high activity and thermostability of OUC-SaLam66 make it a promising candidate for LOS preparation.

Using Poly(amidoamine) PAMAM-βCD Dendrimer for Controlled and Prolonged Delivery of Doxorubicin as Alternative System for Cancer Treatment

Background/Objectives: Doxorubicin (Dox) is an anticancer drug used in the treatment of a wide range of solid tumors; however, Dox causes systemic toxicity and irreversible cardiotoxicity. The design of a new nanosystem that allows for the control of Dox loading and delivery results is a powerful tool to control Dox release only in cancer cells. For this reason, supramolecular self-assembly was performed between a poly(amidoamine) (PAMAM) dendrimer decorated with four β-cyclodextrin (βCD) units (PAMAM-βCD) and an adamantane–hydrazone–doxorubicin (Ad-h-Dox) prodrug. Methods: The formation of inclusion complexes (ICs) between the prodrug and all the βCD cavities present on the surface of the PAMAM-βCD dendrimer was followed by 1H-NMR titration and corroborated by 2D NOESY experiments. A full characterization of the supramolecular assembly was performed in the solid state by thermal analysis (DSC/TGA) and scanning electron microscopy (SEM) and in solution by the DOSY NMR technique in D2O. Furthermore, the Dox release profiles from the PAMAM-βCD/Ad-h-Dox assembly at different pH values was studied by comparing the efficiency against a native βCD/Ad-h-Dox IC. Additionally, in vitro cytotoxic activity assays were performed for the nanocarrier alone and the two supramolecular assemblies in different carcinogenic cell lines. Results: The PAMAM-βCD/Ad-h-Dox assembly was adequately characterized, and the cytotoxic activity results demonstrate that the nanocarrier alone and its hydrolysis product are innocuous compared to the PAMAM-βCD/Ad-h-Dox nanocarrier that showed cytotoxicity equivalent to free Dox in the tested cancer cell lines. The in vitro drug release assays for the PAMAM-βCD/Ad-h-Dox system showed an acidic pH-dependent behavior and a prolonged profile of up to more than 72 h. Conclusions: The design of PAMAM-βCD/Ad-h-Dox consists of a new controlled and prolonged Dox release system for potential use in cancer treatment.

Chemical recycling of polymer contaminated poly(ethylene terephthalate) by neutral hydrolysis

Plastic recycling is gaining traction to reduce the demand for fossil resources for plastic production. Poly(ethylene terephthalate) (PET), mainly used in the packaging and textile sectors, is often isolated in the sinking fraction during the density-based separation of mixed plastic waste streams. The heterogeneity of the sinking fraction makes direct mechanical recycling of PET impossible. Therefore, neutral hydrolysis of PET was investigated in the presence of other polymer contaminants to study their impact on the neutral hydrolysis of PET. PA6, PC, POM, and PVC were found to decompose during hydrolysis, whereas ABS, PMMA and a mixture of PE, PP and PS was chemically inert during the hydrolysis treatment. The subsequent BHET synthesis with excess ethylene glycol was performed directly on a mix of the polymer contaminated hydrolysis products or a hydrolyzed post-consumer plastic waste fraction. BHET was successfully formed in the plethora of decomposition products in the synthesis, and a subsequent recrystallization recovered the BHET in high purity with only water being used as solvent. This demonstrated a robust method to handle PET fractions in mixed plastic waste that can be applied without purification prior to BHET synthesis – enabling chemical recycling of PET.Abbreviations: ABS, Poly(acetonitrile-butadiene-styrene); ATR-FTIR, Attenuated Total Reflectance Fourier Transformed Infrared Spectroscopy; BC, Bis(2-Hydroxyethyl) terephthalate crystals; BHET, Bis(2-Hydroxyethyl) terephthalate; DMSO, Deuterated dimethyl sulfoxide; DSC, Differential Scanning Calorimetry; EG, Ethylene glycol; 1H NMR, Proton Nuclear Magnetic Resonance; Hm, Melting enthalpy; Oligo, Oligomers; PA6, Polyamide 6; PC, Polycarbonate; PE, Polyethylene; PET, Poly(ethylene terephthalate); PMMA, Poly(methyl methacrylate); POM, Polyoxymethylene; PP, Polypropylene; PS, Polystyrene; P, Purity; PVC, Poly(vinyl chloride); rpm, Revolutions per minute; SPHP, Solid Phase Hydrolysis Product; Ti(IV)OBu, Titanium(IV) butoxide; Tm, Melting temperature; TPA, Terephthalic acid; Wt, Weight; Y, Solid Phase Hydrolysis Product yield; Yt, Bis(2-Hydroxyethyl) terephthalate yield; ν, IR stretching mode; δ, IR bending mode; ω, IR wagging mode.

Distinct lignocelluloses of plant evolution are optimally selective for complete biomass saccharification and upgrading Cd2+/Pb2+ and dye adsorption via desired biosorbent assembly

In this study, 15 plant species representing plant evolution were selected, and distinct lignocellulose compositions for largely varied biomass enzymatic saccharification were detected. By comparison, the acid-pretreated lignocellulose of rice mutant was of the highest Congo-red adsorption (298 mg/g) accounting for cellulose accessibility, leading to complete cellulose hydrolysis and high bioethanol production. By conducting oxidative-catalysis with the acid-pretreated lignocellulose of moss plant, the optimal biosorbent was generated with maximum Cd/Pb adsorption (54/118 mg/g), mainly due to half-reduced cellulose polymerization degree and raised functional groups accountable for multiple physical and chemical interactions. Furthermore, the acid-pretreated lignocellulose of eucalyptus was of large and small pores for much higher adsorption capacities with direct-yellow and direct-blue than those of the previously-reported. Therefore, this study raises a mechanism model about how distinct lignocelluloses of plant evolution are selective for complete biomass saccharification and optimal biosorbents assembly, providing insights into lignocellulose biosynthesis and biomass conversion.

Maleic Acid-Butanol Pretreatment to Enhance Cellulose Accessibility for Enzymatic Hydrolysis and Ethanol Production from Oil Palm Empty Fruit Bunch

Maleic Acid-Butanol Pretreatment to Enhance Cellulose Accessibility for Enzymatic Hydrolysis and Ethanol Production from Oil Palm Empty Fruit Bunch

Correction: Production of Hydrolysates from Swordfish (Xiphias gladius) Head Muscle as New Protein Source: Evaluation of Nutritional, Antioxidant and Functional Properties

Correction: Production of Hydrolysates from Swordfish (Xiphias gladius) Head Muscle as New Protein Source: Evaluation of Nutritional, Antioxidant and Functional Properties

Synergistic effect of Lewis acid-base sites in Zr4+-doped layered double hydroxides promotes rapid decontamination of nerve and blister agents under ambient conditions

Nerve and blister agents are among the deadliest chemicals posing a major threat to the society, and the development of materials that can rapidly decontaminate them under solvent-free ambient conditions is a major societal challenge. In this paper, layered double hydroxides (ZnAlxZr1−x-LDH) with varying Zr4+ doping content were synthesized and the decontamination properties of nerve and blister agents were investigated under ambient conditions. The results show that, compared to ZnAl-LDH, the ZnAl0.4Zr0.6-LDH with the highest amount of Zr4+ dopant reduced the decontamination reaction half-life of sarin (GB) and soman (GD) by 10 and 9 times, respectively. Mechanism studies revealed that ZnAl0.4Zr0.6-LDH employs the synergistic effect of Lewis acid-base sites to catalyze the decomposition of GB and GD into hydrolysis products and surface-bound hydrolysis products. The study also showed that under ambient conditions, ZnAl0.4Zr0.6-LDH demonstrated superior decontamination performance for the sulfur mustard (HD) simulant 2-chloroethyl ethyl sulfide (CEES) compared to ZnAl-LDH, effectively catalyzing the detoxification of CEES into dehydrohalogenation (EVS) and 1,2-bis-(ethylthio) ethane (BETE). ZnAl0.4Zr0.6-LDH also had satisfactory decontamination performance against HD. This work provides not only a green and efficient catalyst with potential for practical applications but also new insights for constructing broad-spectrum, highly efficient self-detoxifying materials.

Conversion of Penta‐Acetyl‐Xylitol to 3‐Acetoxymethylene‐Tetrahydrofuran by a Combined Hetero‐/Homogeneous Tandem Catalyst System

A tandem catalyst system comprised of trifluoromethanesulfonic (triflic acid, HOTf) or Hafnium tetratriflate (Hf(OTf)4) and Ru/C in glacial acetic acid (HOAc) as the solvent at 200 °C and ~ 7 MPa hydrogen pressure in a batch reactor converts penta‐acetyl‐xylitol ((2R,3R,4S)‐Pentane‐1,2,3,4,5‐penta‐acetoxy‐pentane) or unprotected xylitol to 3‐acetoxymethylene‐tetrahydrofuran (3‐AMT) in up to 15 % yield at full conversion. A comparative analysis by SEM‐EDS and XPS of the fresh commercial Ru/C catalyst vs catalyst reused and recovered after 5 cycles shows increasing aggregation of ruthenium to larger particles with a concomitant decrease in yield of 3‐AMT to 8‐9 % for cycles 4 and 5. 3‐AMT or its hydrolysis product 3‐hydroxymethyl‐tetrahydrofuran (3‐HMT) are valuable synthons for the preparation of agrochemicals, pharmaceuticals and specialty polyurethanes and polyesters.

Spatial and Temporal Visualization of Polymorphic Transformations in Pharmaceutical Tablets.

X-ray Diffraction Computed Tomography (XRD-CT) represents a cutting-edge method for non-destructive material analysis, offering the unique capability of providing molecular-level information with spatial resolution. In this study, we have applied XRD-CT to investigate pharmaceutically relevant tablets that have been subjected to a range of compression pressures typical in tablet manufacturing. By employing XRD-CT to pharmaceutical tablets, we reveal material changes without tablet destruction, thereby avoiding potential phase transformations during sample preparation that could lead to errors in the interpretation of the processes that have occurred. Utilizing a pressure-sensitive marker, glycolide, we have tracked changes within tablet structures induced by compression, pinpointing locations where glycolide undergoes pressure-induced transformation. Additionally, we conducted a follow-up study with analysis one month later, observing an in-situ hydrolysis reaction of glycolide within the tablets. Through the complementary use of electron diffraction, we have elucidated the structure of the hydrolysis product, further enhancing our understanding of temporal changes in the tablets.