Powder Diffraction Research Articles

Investigation of Stabilized Amorphous Solid Dispersions to Improve Oral Olaparib Absorption.

In this study, we investigated the formulation of stable solid dispersions to enhance the bioavailability of olaparib (OLA), a therapeutic agent for ovarian cancer and breast cancer characterized as a BCS class IV drug with low solubility and low permeability. Various polymers were screened based on solubility tests, and OLA-loaded solid dispersions were prepared using spray drying. The physicochemical properties of these dispersions were investigated via scanning electron microscopy (SEM), differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD), and Fourier Transform Infrared Spectroscopy (FT-IR). Subsequent dissolution tests, along with assessments of morphological and crystallinity changes in aqueous solutions, led to the selection of a hypromellose (HPMC)-based OLA solid dispersion as the optimal formulation. HPMC was effective at maintaining the supersaturation of OLA in aqueous solutions and exhibited a stable amorphous state without recrystallization. In an in vivo study, this HPMC-based OLA solid dispersion significantly enhanced bioavailability, increasing AUC0-24 by 4.19-fold and Cmax by more than 10.68-fold compared to OLA drug powder (crystalline OLA). Our results highlight the effectiveness of HPMC-based solid dispersions in enhancing the oral bioavailability of OLA and suggest that they could be an effective tool for the development of oral drug formulations.

Investigation on the Drug Release Efficacy of the Ibuprofen-Loaded ZIF-8/Fe3O4 NPs Nanocarrier.

In this work, a one-pot multicomponent synthesis of the ibuprofen-loaded Fe3O4 nanoparticles-supported zeolitic imidazolate framework-8 (Ibu-ZIF-8/Fe3O4 NPs) nanohybrid was carried out. The ZIF-8/Fe3O4 NPs nanohybrid was used as a drug carrier for the in vitro release of ibuprofen in a PBS solution. The structure and morphology of the synthesized materials were investigated by powder X-ray diffraction (PXRD) analysis, transmission electron microscopy (TEM) analysis, UV-visible absorption studies, FTIR spectroscopy, and thermogravimetric analysis (TGA). The ibuprofen release kinetics was studied by UV-visible spectroscopy. The mechanism of drug delivery was thoroughly investigated and the Higuchi model was found as the best-fitted model for the ibuprofen release study. The 20 wt % Fe3O4 NPs-supported ZIF-8 nanohybrid exhibited more than 95% ibuprofen release efficiency in phosphate buffer saline of pH 7.4 within 2 h. The separation ability of the nanohybrid was very good, and it was easily separated by a simple commercial magnet. In order to investigate the cell viability, the cytotoxicity of ZIF-8, Fe3O4 NPs, and ZIF-8/20 wt % Fe3O4 NPs was investigated using MTT assays against Leishmania donovani promastigotes. The ZIF-8/20 wt % Fe3O4 NPs nanohybrid carrier exhibited a cell growth inhibition effect with a high correlation coefficient and low probability (p) values. The high release of drug molecules may be due to the more open site of the ZIF-8/Fe3O4 NPs nanohybrid. The drug release profile suggests that the nanohybrid can be potentially used as a drug carrier for targeted drug delivery systems.

Hexagonal rod-like Eu3+doped CaMoO4 phosphors: Structural, photoluminescence and photometric properties for display device applications

A multicolored LED illumination device is a compact, durable, easy to obtain color-adjustable output illumination source. It is frequently utilized in the domains of room illumination and exterior displays. However, the advancement of multicolor LEDs has been hampered by the rise in price and the fall in luminous efficacy while changing illumination colors. In the present investigation we have prepared intense red emitting Eu3+ doped CaMoO4 phosphor nanopowders via simple solid-state reaction technique. The powder X-ray diffraction (PXRD) studies reveal the crystalline nature of the samples with scheelite–type mono phase tetragonal structure with I41/a space group. The band gap (Eg) energy values were estimated and found to range between 4.63–5.32 eV. Scanning electron microscopy (SEM) studies reveled the hexagonal rod-like structures with different Aloe Vera gel concentrations. The particle size was found to be around 40 nm. The vibrational modes of the prepared powders were evaluated by using Fourier Transform Infrared Spectroscopy (FTIR) and Raman spectroscopy. It was observed from the results that, there were 26 vibrational modes of CaMoO4 (Γ=3Ag + 5Au + 5Bg + 3Bu + 5Eg + 5Eu) 8 of which (4Au and 4Eu) were infrared active and 13 (Ag, Bg, and Eg) are Raman active. Photoluminescence (PL) emission intensity increases up to 5 mol% of Eu3+ ions load and subsequently it declines due to the concentration quenching phenomenon and effective energy transfer from Mo-O charge transfer band (CTB) to 5D0 levels of Eu3+. It was noticed from PL emission spectra that, four intense peaks located at 5D0 → 7F1 (590 nm), 5D0 → 7F2 (613 nm), 5D0 → 7F3 (654 nm), 5D0 → 7F4 (702 nm) of Eu3+ respectively. The Commission International de I'Eclairage (CIE) diagram indicates the red color emission and average correlated color temperature (CCT) value was found to be 2050 K. Further, the external quantum efficiency (QE) and color purity (CP) were calculated to check the phosphor efficiency and found to be 92% and 72% respectively. The present investigation opens up a new avenue in the fabrication of low-cost display devices with high color purity and luminous efficacy.

Spectroscopic properties of Pr3+-doped Titania-Silicate glass ceramic for photonic applications

Silicate-Titania (SiTi) glass-ceramics doped with Pr3+ (0.6, 1.6, 2.4 and 3.6 mol%) ions were prepared by sol-gel technique. The materials were characterized by powder XRD, FTIR, TEM, EDX, Optical absorption and Photoluminescence spectroscopy. The identification of non-bridging oxygen (NBO) formation and the removal of OH groups are validated through analysis of the FTIR spectra. Additionally, measurements using XRD and TEM showed that the samples contain nano-sized crystallites. The three phenomenological Judd–Ofelt (J–O) intensity parameters Ω2, Ω4, and Ω6 were obtained and used to analyze different radiative characteristics for the fluorescence levels of Pr3+ in the glass ceramic, including radiative lifetime, branching ratio, radiative transition probability and stimulated emission cross-section. Several emissions were observed in the visible region, among which the 1D2→3H4 in the orange-red region is the most intense. All of these reported branching ratios, stimulated emission cross-sections, and visible emission spectra point to the possibility of employing them as red region lasers. The CIE chromaticity coordinates from all of the emission spectra were also assessed to determine if these materials are suitable for orange-red phosphors. According to CIE chromaticity investigations, 1.6 mol% of Pr3+ ion concentration is ideal for SiTiPr glass-ceramic for use as red phosphors and possibly red lasers.

Intermediate valence behavior of the ternary cerium-nickel-phosphide Ce2Ni12P5

The crystal structure of the ternary phosphide Ce2Ni12P5 (La2Ni12P5-type structure) has been determined from X-ray powder diffraction data: full profile refinement, monoclinic symmetry, space group P21/m, a = 10.7809(2) Å, b = 3.6869(1) Å, c = 13.1490(3) Å, β = 107.776(4)º, RI = 0.068, RP = 0.044, RwP = 0.060. Ce2Ni12P5 is a ferromagnet with a Curie temperature of 5.8(5) K. A significant deviation from the linearity of the temperature dependence of the electrical resistance for Ce2Ni12P5 has been found. The low-temperature part of the electrical resistance indicates the presence of magnetic interactions in Ce2Ni12P5. The influence of a magnetic field on the electrical resistance of Ce2Ni12P5 has been studied. The X-ray absorption spectrum at the Ce LIII edge and X-ray emission spectra of Ni and P at the K and LIII edges have been studied experimentally and theoretically using DFT+U calculations. The calculations show good agreement with the experimental measurements. The effective valence of Ce in Ce2Ni12P5 determined based on the Ce LIII absorption spectrum is ϑeff ∼ 3.05.

Recycling of additively printed anisotropic Nd-Fe-B bonded magnets

A high potential cost-effective and environmentally friendly method has been applied for recycling anisotropic Nd-Fe-B bonded magnets. Waste additively printed Hydrogenation-Disproportionation-Desorption-Recombination (HDDR) Nd-Fe-B anisotropic bonded magnet was pulverized into composite powder containing Nd-Fe-B particles and nylon binder through cryomilling at a liquid nitrogen temperature (∼77 K) under Ar inert atmosphere. Then, the cryomilled composite powder was warm compacted into a bonded magnet. The magnetic particles were aligned during post-compaction annealing under a magnetic field of 30 kOe. The recycled bonded magnets have a higher density (3 % enhancement), but slightly inferior magnetic properties compared to the original magnets, i.e., the magnetic remanence, coercivity and maximum energy product are reduced by 2 %, 3 % and 8 %, respectively. The scanning electron microscopy revealed that some HDDR Nd-Fe-B powder crumbled into fine particles during cryomilling. Powder X-ray diffraction showed a small amount of Nd-oxide impurity in the cryomilled powder. The slightly deteriorated magnetic properties are ascribed to the oxidation of Nd-Fe-B particles due to formation of fresh fracture surface during cryomilling. The approach enables the direct reuse of end-of-life bonded magnets in an economical and environmentally friendly way.

Crystal structure and characterization of monascin from the extracts of Monascus purpureus-fermented rice.

We present a novel solid form of monascin, an azaphilonoid derivative extracted from Monascus purpureus-fermented rice. The crystal structure, C21H26O5, was characterized by single-crystal X-ray diffraction and belongs to the orthorhombic space group P212121. To gain insight into the electronic properties of the short contacts in the crystalline state of monascin, we utilized the Experimental Library of Multipolar Atom Model 2 (ELMAM2) database to transfer the electron density of monascin in its crystalline state. Hirshfeld surface analysis, fingerprint analysis, electronic properties and energetic characterization reveal that intermolecular C-H...O hydrogen bonds play a crucial role in the noncovalent bonding interactions by connecting molecules into two- and three-dimensional networks. The molecular electrostatic potential (MEP) map of the monascin molecule demonstrates that negatively charged regions located at four O atoms are favoured binding sites for more positively charged amino acid residues during molecular recognition. In addition, powder X-ray diffraction confirms that no transformation occurs during the crystallization of monascin.

High-temperature heat treatment of hydrogen-reduced bauxite residue-calcite pellets for iron particles growth and separationTraitement thermique à haute température de boulettes de résidus de bauxite et calcite réduites à l’hydrogène pour la croissance et la séparation des particules de fer

ABSTRACT Bauxite residue characterised as a polymetallic source containing iron, alumina, titanium, calcium, silicon and rare earth elements offers an opportunity for reduced waste volume and the recovery of valuable metals. This study focuses on the agglomeration of bauxite residue with calcite, followed by hydrogen reduction at 1000°C. The resulting iron particles in the reduced pellets were initially very small distributed in a porous oxide matrix, posing challenges for physical separation methods. To address this issue, further heat treatments were conducted on the reduced pellets in an argon atmosphere, ranging from 1100°C to 1550°C. Phase analysis and microstructural examinations were performed using X-ray powder diffraction and scanning electron microscopy, respectively. Experimental findings indicate that the size of iron particles in the reduced pellets increases with higher heat treatment temperatures. Up to 1200°C, the oxide matrix remains a solid state, transitioning to a semi-molten and molten state above this heat treatment temperature and complete separation of iron from the oxide matrix above 1500°C. An alkali-leachable phase is present in the reduced pellets, initially in the form of calcium aluminate (mayenite), while above 1400°C, this phase dissociates to form monocalcium aluminate, and complete conversion at 1500°C. As observed in the microstructural analysis, there is an increase in the particle size of iron in both the solid and semi-molten states with an increasing in temperature from 1100°C up to 1300°C. This comprehensive study sheds light on the transformative effects of varying heat treatment temperatures on the composition and microstructure of bauxite residue-based materials.

Thiocarbonyl Pseudohalides - The Curious Case of Thiocarbonyl Dithiocyanate.

Thiocarbonyl dithiocyanate (1) and chlorothiocarbonyl thiocyanate (2) were synthesized from thiophosgene and ammonium or silver thiocyanate, respectivley. Their crystal structures show syn-anti (1) and syn (2) conformations, which were confirmed in the bulk phases by powder X-ray diffraction, vibrational spectroscopy and DFT calculations. Further calculations explain the isolation of the kinetic reaction products by a lower transition states opposed to the thermodynamic reaction products. Reaction of 1 with ethanol gave a dithiobiuret derivative (3). In a proof-of-principle study we show that it in turn can be used for the complexation of nickel to yield (4).

Hybrid Ethylcellulose Polymeric Films: Ag(I)-Based Components and Curcumin as Reinforcing Ingredients for Enhanced Food Packaging Properties.

Bio-active ethylcellulose (EC) polymeric films have been obtained by incorporating curcumin (curc) and Ag(I)-based compounds, known for their antioxidant and antimicrobial activity, respectively, within the polymeric matrix. The recently reported Ag(I) coordination polymer, in both its structural forms (α-[(bpy)Ag(OTf)]∞ and β-{[(bpy)Ag][OTf]}∞), and the [(bpy)Ag(OTf)]∞-curc polymeric co-crystal (bpy=2,2'-bipyridine; OTf=trifluoromethanesulfonate) have been selected as Ag(I) species. The hybrid composite films have been prepared through the simple solvent casting method and characterized through Powder X-Ray Diffraction (PXRD), Differential Scanning Calorimetry (DSC) and Fourier Transform Infrared (FTIR) spectroscopy, Scanning Electron Microscope (SEM), UV-vis spectroscopy. The deep investigation of the film samples highlighted the non-inert behaviour of EC towards these specific active ingredients. Antimicrobial tests showed that EC films embedding the Ag(I)-based compounds present good antimicrobial performance, in particular against Staphylococcus aureus, used as a model of Gram-positive bacteria. In addition, Silver migration tests, performed on the Ag(I)-incorporating EC films, evidenced low values of silver release particularly in the case of the EC films incorporating [(bpy)Ag(OTf)]∞-curc.

Ruthenium(II) Complex-Based Tetradentate Schiff Bases: Synthesis, Spectroscopic, Antioxidant, and Antibacterial Investigations.

In this work, we describe the synthesis of novel Ruthenium (II) complex-based salen Schiff bases. The obtained Ruthenium (II) complexes are characterized using usual spectroscopic and spectrometric techniques, viz., IR, UV-Vis, NMR (1H and 13C), powder X-ray diffraction, and HRMS. Further techniques, such as DTA-TGA and elemental analysis, are used to well establish the structure of the obtained complexes. Octahedral geometries are tentatively proposed for the new Ru(II) complexes. The measured molar conductance for the Ruthenium (II) complexes shows their electrolytic nature (4.24-4.44 S/m). The new Ru(II) complexes are evaluated for their antioxidant and antibacterial activities. The DPPH radical scavenging, FRAP, and total antioxidant capacity (TAC) assays show that the obtained complexes are more potent than the used positive control. They also exhibit promising antibacterial responses against pathogen bacteria: [RuH2L3Cl2] exhibits an important inhibition against Bacillus subtilis DSM 6633, with an inhibition zone of 21 ± 1.41 mm with an MIC value of 0.39 mg/mL, and Proteus mirabilis INH, with 16.50 ± 0.70 mm and an MIC value of 0.78 mg/mL, while [RuH2L2Cl2] exerts interesting antibacterial effects versus Bacillus subtilis DSM 6633 (21 ± 1.41 mm) and Proteus mirabilis INH (25.5 ± 0.70 mm) with equal MIC values of 0.97 mg/mL.

Energy-safety balanced composites of attractive cyclic nitramines with polyaniline

Composite microcrystals of the cyclic nitramines 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane (ε-CL-20), 1,3,5-trinitro-1,3,5-triazinane(RDX), 1,3,5,7-tetranitro-1,3,5,7-tetrazocane (β-HMX), and cis-1,3,4,6-tetranitrooctahydroimidazo-[4,5-d]imidazole (BCHMX) with polyaniline (PANi) have been prepared and thoroughly characterized in terms of morphology and phase purity. PANi outperformed other conducting polymers in terms of selectivity towards NAs due to its better interaction with NAs, low production cost, and ease of preparation. The bonding of nitramines with the polymeric PANi chain has been examined by means of Fourier transform infrared (FTIR), Raman spectroscopy methods, and fluorescence quenching; the Raman spectrum has shown the laser sensitivity of these microcrystals. Powder X-ray diffraction results have shown changes in polymorph modifications in CL20 (from ɛ to β) and HMX (from β to α) during the preparation of the composites, which have also been confirmed by spectral and differential thermal analysis techniques. The structural orientations found in these composites significantly stabilize nitramines against impact; their detonation properties have slightly deteriorated, but the PANi electrical conductivity has strongly increased their electric-spark sensitivity. The above properties of the prepared composites determine their potential use mainly as parts of the electric or laser impulse initiators, having “a green character”, for various charges.

Photocatalytic Degradation of Organic Dyes by Magnetite Nanoparticles Prepared by Co-Precipitation.

Iron oxide nanoparticles were synthesized by co-precipitation using three different iron salt stoichiometric mole ratios. Powder X-ray diffraction patterns revealed the inverse cubic spinel structure of magnetite iron oxide. Transmission electron microscopic images showed Fe3O4 nanoparticles with different shapes and average particle sizes of 5.48 nm for Fe3O4-1:2, 6.02 nm for Fe3O4-1.5:2, and 6.98 nm for Fe3O4-2:3 with an energy bandgap of 3.27 to 3.53 eV. The as-prepared Fe3O4 nanoparticles were used as photocatalysts to degrade brilliant green (BG), rhodamine B (RhB), indigo carmine (IC), and methyl red (MR) under visible light irradiation. The photocatalytic degradation efficiency of 80.4% was obtained from Fe3O4-1:2 for brilliant green, 61.5% from Fe3O4-1.5:2 for rhodamine B, and 77.9% and 73.9% from Fe3O4-2:3 for both indigo carmine and methyl red. This indicates that Fe3O4-2:3 is more efficient in the degradation of more than one dye. This study shows that brilliant green degrades most effectively at pH 9, rhodamine B degrades best at pH 6.5, and indigo carmine and methyl red degrade most efficiently at pH 3. Recyclability experiments showed that the Fe3O4 photocatalysts can be recycled four times and are photostable.

Polymethylenetetrazole: Synthesis, Characterization, and Energetic Properties.

The tetrazole moiety remains one of the most interesting scaffolds in the development of new high-energy density materials (HEDMs) because of its desired characteristics, such as high nitrogen content and heat of formation (HOF). The combination of several heterocycles with high HOF seems to be a promising strategy for obtaining energetic materials with superior properties. Herein, we report the synthesis and characterization of a tetrazole polymer, polymethylenetetrazole (PMT), as a potential HEDM. The compound was characterized using NMR, IR, and Raman spectroscopy. Its weight average molecular mass was obtained by static light scattering (SLS), and its physical properties by powder XRD analysis. The density, sensitivity to friction (FS), and impact (IS) of the compound were determined as well. The results of the thermal and energetic properties of PMT suggest that this polymer could be an insensitive explosive.

Ternary Copper(II) Coordination Compounds with Nonpolar Amino Acids and 2,2′-Bipyridine: Monomers vs. Polymers

Reactions of copper(II) sulfate with 2,2′-bipyridine (bipy) and amino acids with nonpolar side chains (l-alanine (HAla), l-valine (HVal), or l-phenylalanine (HPhe)) were investigated under different solution-based and mechanochemical methods. Five new ternary coordination compounds were obtained by a solution-based synthesis and three of them additionally by the liquid-assisted mechanochemical method: {[Cu(μ-l-Ala)(H2O)(bipy)]2SO4·2H2O}n (1a·2H2O), {[Cu(μ-l-Ala)(H2O)(bipy)][Cu(l-Ala)(H2O)(bipy)]SO4·2.5H2O}n (1b·2.5H2O), {[Cu(μ-l-Val)(H2O)(bipy)][Cu(l-Val)(H2O)(bipy)]3(SO4)2·4H2O}n (2·4H2O), [Cu(l-Phe)(H2O)(bipy)][Cu(l-Phe)(SO4)(bipy)]∙8H2O (3·8H2O), and [Cu(l-Phe)(H2O)(bipy)][Cu(l-Phe)(SO4)(bipy)]∙9H2O (3·9H2O). The compounds were characterized by single-crystal and powder X-ray diffraction, infrared spectroscopy, and a thermal analysis. Structural studies revealed two structural types, monomeric in 3·8H2O and 3·9H2O, polymeric architectures in 1a·2H2O, and mixed structures (monomeric and polymeric) in 1b·2.5H2O and 2·4H2O. The copper(II) ion is either pentacoordinated or hexacoordinated, with an observed Jahn–Teller effect. The crystal structures are based on an intensive network of hydrogen bonds and π interactions. 1a·2H2O and 2·4H2O showed substantial in vitro antiproliferative activity toward human hepatocellular carcinoma (HepG2) and moderate activity toward human acute monocytic leukemia cell lines (THP-1).

A stable and regenerative TiO2/Bi2MoO6 photocatalyst for highly effective degradation of Rhodamine B and Congo Red

ABSTRACT This research unravels a facile method for synthesising TiO2/Bi2MoO6 photocatalysts and their effective applications in degrading industrial dyes. Initially, Bi2MoO6 was prepared as the substrate, followed by the addition of TiO2 to form the TiO2/Bi2MoO6 composite. The photocatalyst was characterised by powder X-ray diffraction (XRD), scanning electron microscopy with energy-dispersive X-ray spectrometry (SEM-EDS), X-ray photoelectron spectroscopy (XPS), high-resolution transmission electron microscopy (HR-TEM), photoluminescence (PL), and UV-Vis diffuse reflectance spectroscopy (UV-Vis DRS). Its photocatalytic properties were evaluated by dye degradation under various conditions, including different dopant loading amounts, the reaction time, the initial concentration of the dye, and pH values. The results indicated that 50 mg of 15% TiO2/Bi2MoO6 achieved the highest photodegradation efficiency: 98.51% for 50 mL 10 mg L−1 Rhodamine B (RhB) within 100 min in a neutral buffer solution and 90.71% for 50 mL 10 mg L−1 Congo Red (CR) within 80 min in an aqueous solution. This material exerted effectiveness across a wide pH range, with removal rates of RhB exceeding 95.41% in both acidic and alkaline conditions. The degradation process conformed to the pseudo-first-order kinetic model. Radical trapping experiments revealed that the dye degradation mechanism involved ∙ O 2 − and h+. Notably, the synthesised TiO2/Bi2MoO6 photocatalyst demonstrated high stability and reusability, maintaining performance even after four degradation cycles. The TiO2/Bi2MoO6 photocatalyst, with TiO2 as the dopant and Bi2MoO6 as the substrate, demonstrated significant versatility and potential for practical dye degradation applications.

Preparation and Evaluation of Clarithromycin Taste-Masking Dry Suspension Using Hot Melt Extrusion Based on Solid Dispersion Technology.

Clarithromycin (CLA) is the preferred drug for treating respiratory infections in pediatric patients, but it has the drawbacks of extreme bitterness and poor water solubility. The purpose of this study was to improve solubility and mask the extreme bitterness of CLA. We use Hot Melt Extrusion (HME) to convert CLA and Eudragit® E100 into Solid Dispersion (SD). Differential scanning calorimetry (DSC) and Powder X-ray diffraction (PXRD) were used to identify the crystalline form of the prepared SDs, which showed that the crystalline CLA was converted to an amorphous form. At the same time, an increase in dissolution rate was observed, which is one of the properties of SD. The results showed that the prepared SD significantly increased the dissolution rate of crystalline CLA. Subsequently, the SD of CLA was prepared into a dry suspension with excellent suspending properties and a taste-masking effect. The bitterness bubble chart and taste radar chart showed that the SD achieved the bitter taste masking of CLA. Principal components analysis (PCA) of the data generated by the electronic tongue showed that the bitter taste of CLA was significantly suppressed using the polymer Eudragit® E100. Subsequently, a dry suspension was prepared from the SD of CLA. In conclusion, this work illustrated the importance of HME for preparing amorphous SD of CLA, which can solve the problems of bitterness-masking and poor solubility. It is also significant for the development of compliant pediatric formulations.

Precise Pore Engineering of Zirconium Metal-Organic Cages for One-Step Ethylene Purification from Ternary Mixtures.

One-step purification of ethylene from ternary mixtures (C2H2, C2H4, and C2H6) can greatly reduce the energy consumption of the separation process, but it is extremely challenging. Herein, we use crystal engineering and reticular chemistry to introduce unsaturated bonds (ethynyl and alkyne) into ligands, and successfully design and synthesized two novel Zr-MOCs (ZrT-1-ethenyl and ZrT-1-alkyne). The introduction of carbon-carbon unsaturated bonds provides abundant adsorption sites within the framework while modulating the pore window size. Comprehensive characterization techniques including single crystal and powder X-ray diffraction, as well as electrospray ionization time-of-flight mass spectrometry (ESI-TOF-MS) confirm that ZrT-1-ethenyl and ZrT-1-alkyne possess an isostructural framework with ZrT-1 and ZrT-1-Me, respectively. Adsorption isotherms and breakthrough experiments combined with theoretical calculations demonstrate that ZrT-1-ethenyl can effectively remove trace C2H2 and C2H6 in C2H4 and achieve separation of C2H2 from C2H4 and CO2. ZrT-1-ethenyl can also directly purify C2H4 in liquid solutions. This work provides a benchmark for MOCs that one-step purification of ethylene from ternary mixtures.

Vitamin B3 Intercalated in Layered Double Hydroxides: A Drug Delivery System for Metabolic Regulation.

The organic compound niacin or nicotinic acid, also known as vitamin B3 (VitB3), is essential for human nutrition and metabolic regulation. However, in high doses, it can provoke side effects, such as hyperglycemia, liver damage, and flushing. Development of a controlled release system that slowly releases VitB3 into the organism would avoid high dosing peaks, thus contributing to decrease the occurrence of side effects in nutritional supplementation. Here, we show that the slow and controlled release of VitB3 in an acid environment can be achieved via its intercalation in layered double hydroxides (LDHs). The synthesis of a ZnAl-VitB3 system is shown, in which VitB3 is intercalated in a ZnAl LDH. The presence of VitB3 in the ZnAl-VitB3 system was confirmed by elemental analysis, infrared (FTIR) and NMR spectroscopy, while successful intercalation in the LDHs was revealed by powder X-ray diffraction (PXRD). In vitro release tests were carried out in a concentrated HCl solution of pH 1.5, a pH similar to the human stomach environment. The results showed a steady release of VitB3 from the LDH host, with 90% of the vitamin liberated in the first 60 min after the suspension of the LDH in the acidic solution.

The Continuous and Reversible Transformation of the Polymorphs of an MGAT2 Inhibitor (S-309309) from the Anhydrate to the Hydrate in Response to Relative Humidity.

Polymorphic control is vital for the quality control of pharmaceutical crystals. Here, we investigated the relationship between the hydrate and anhydrate polymorphs of a monoacylglycerol acyltransferase 2 inhibitor (S-309309). Solvent evaporation and slurry conversion revealed two polymorphs, the hydrate and the solvate. The solvate was transformed into the hydrate by heating. X-ray powder diffraction demonstrated that the hydrate was transformed into an anhydrate via an intermediate state when heated. These crystal forms were confirmed under controlled humidity conditions; the presence of the anhydrate, the intermediate hydrate, or the hydrate depended on the relative humidity at 25 °C. The stoichiometry of S-309309 in water in the hydrate form was 4:1. The hydrates and anhydrates exhibited similar crystal structures and stability. The water of hydration in the intermediate hydrate was 0.1-0.15 mol according to the dynamic vapor sorption profile. The stability and dissolution profile of the anhydrate and hydrate showed no significant change due to similar crystal lattices and quick rehydration of the anhydrate. A mechanism for the reversible crystal transformation between the anhydrate and pseudo-polymorphs of the hydrate was discovered. We concluded that S-309309 causes a pseudo-polymorphic transformation; however, this is not a critical issue for pharmaceutical use.