Ground Mixture Research Articles

Solvent-Free Synthesis of HKUST-1 with Abundant Defect Sites and Its Catalytic Performance in the Esterification Reaction of Oleic Acid.

HKUST-1 has received increasing attention because of its potential applications in many fields, such as heterogeneous catalysis, sensors, gas storage, and separation. Herein, we report that HKUST-1 can be facilely prepared by heating a ground mixture of copper nitrate trihydrate and 1,3,5-benzenetricarboxylic acid in an autoclave at 80 °C for 10 h. The data from nitrogen sorption show that the obtained material, named HKUST-1-free, possesses a high BET specific surface area of 1671 m2/g and a pore volume of 0.8 cm3/g. The results from acid-base titration indicate that the number of defect sites in HKUST-1-free is more than that in HKUST-1-solvent prepared by the solvothermal method. As a heterogeneous catalyst, HKUST-1-free gave a high yield (91%) of methyl oleate in the esterification reaction of oleic acid with methanol at room temperature compared to HKUST-1-solvent (70%). Additionally, it is proven that HKUST-1-free is a heterogeneous catalyst and can be reused.

The influence of herbicide protection on the yield of annual sunflower (Helianthus annuus L.) in the conditions of Western Forest Steppe

Methods. Field, quantitative to determine weediness of crops, mathematical and statistical to assess the reliability of the data obtained.
 Results. It was established that the species composition of the dicot segetal vegetation in the sunflower agrocenosis was mainly represented by white quinoa (Chenopodium album L.), common bittersweet (Amaranthus retroflexus L.), birch mustard (Polygonum convolvulus L.), field mustard (Sinapis arvensis L.). Among the variants of the experiment, the highest number of weeds was noted in the control without herbicides — 31.2 weeds/ m2. The introduction of soil and insurance herbicides contributed to the reduction of weediness of sunflower crops. The negative influence of segetal vegetation on the formation of the yield of the studied crop has been proven, which manifested itself in a decrease of its seed productivity with an increase in the number of weeds in the crops. Thus, in the control variant without the use of herbicides the yield of sunflower was the lowest and amounted to 1.55 t/ ha due to strong weediness of the crops. The highest yield of sunflower (4.13 t/ ha) was noted for the variant in which the herbicide Oscar Premium, s.e. was applied to the seedlings. at the rate of 3.75 l/ ha and post-emergence spraying of crops with a tank mixture of herbicides Challenge, s.c., 1.0 l/ ha and Heliantex, s.c., 0.045 l/ ha with the addition of Vivolt surfactant 0.25 l/ ha.
 Conclusions. The lowest weediness of sunflower agrocenoses (1.5 units/ m2) at the time of harvesting was noted on the variant with the use of ground (Oscar Premium, s.e. 3.75 l/ ha) and tank mixture of insurance herbicides (Challenge, s.c., 1.0 l/ ha + Heliantex, s.c., 0.045 l/ ha + Vivolt surfactant 0.25 l/ ha) in the phase of BBCH 14. The highest yield of the researched crop was also noted on the specified version of the experiment — 4.13 t/ ha, which is 2.58 t/ ha more than the control version.

Preparation, solubility, and anti-inflammatory effects of a complex of diphenylcyclopropenone/β-cyclodextrin derivatives as the treatment of alopecia areata.

To investigate the preparation of inclusion complexes of diphenylcyclopropenone (DPCP)/β-cyclodextrin (β-CD) derivatives using a three-dimensional (3D) ball mill, and verify the inclusion behavior of the solid dispersion. Additionally, we aimed to investigate the effect of DPCP/β-CDs complex formation on the spleens of male C57BL/6 mice in terms of anti-inflammatory effects. The inclusion complexes of DPCP with β-CD and hydroxypropyl-β-cyclodextrin (HPβCD) were prepared using a 3D ball mill. Powder X-ray diffraction (PXRD) and Fourier-transform infrared spectroscopy (FT-IR) were used to evaluate the solid-state properties. The solubility of the prepared DPCP/β-CD and HPβCD complexes and the intermolecular interaction between DPCP and β-CD derivatives in solution were assessed using 1H nuclear magnetic resonance (NMR). Furthermore, the anti-inflammatory effects of DPCPs in the prepared DPCP/CD complexes were investigated using spleens from male C57BL/6 mice, with measurement of interferon gamma (IFN-γ) secretion as an endpoint. Additionally, the protective effects of each drug on NIH-3T3 cells exposed to ultraviolet (UV) irradiation were examined. Solid-state characterization confirmed the formation of inclusion complexes in the 3D ground mixture (3DGM) (DPCP/β-CD = 1/1) and 3DGM (DPCP/HPβCD = 1/1) complexes through PXRD and IR analysis. The solubility of 3DGM (DPCP/β-CD = 1/1) and 3DGM (DPCP/HPβCD = 1/1) was 17.5μg/mL and 58.4μg/mL, respectively, indicating higher solubility than that of DPCP alone. NMR analysis of 3DGM samples suggested that DPCP/β-CD and DPCP/HPβCD form inclusion complexes at a molar ratio of 1/1 but with different inclusion modes. Regarding the anti-inflammatory activity of DPCP, 3DGM (DPCP/HPβ-CD) showed anti-inflammatory effects at lower doses compared to 3DGM (DPCP/β-CD) in terms of IFN-γ and NIH-3T3 cells injured by UV irradiation. We successfully formed inclusion complexes of DPCP/β-CD and DPCP/HPβCD using the 3D ground mixture method. NMR analysis suggested that DPCP/β-CD and DPCP/HPβCD form inclusion complexes at a molar ratio of 1/1 but with different inclusion modes. The anti-inflammatory activity of DPCP was more pronounced in 3DGM (DPCP/HPβCD) at lower doses compared to that in 3DGM (DPCP/β-CD), indicating that the HPβCD derivatives were more effective in enhancing the anti-inflammatory properties of DPCP.

Characterization, Preparation, and Promotion of Plant Growth of 1,3-Diphenylurea/β-Cyclodextrin Derivatives Inclusion Complexes.

The study aimed to prepare inclusion complexes of 1,3-diphenylurea (DPU) with β-cyclodextrin (βCD) and 2-hydroxypropyl-β-cyclodextrin (HP-βCD) using a three-dimensional ground mixture (3DGM). Their physicochemical properties, intermolecular interactions, solubilities, and plant growth-promoting activities were investigated on broccoli sprouts. Phase-solubility diagrams indicated the stability constant (Ks) and complexation efficiency (CE) of βCD/DPU were found to be K1/1 = 250 M-1, CE = 2.48× 10-3. The Ks and CEs of HP-βCD/DPU were found to be K1/1 = 427 M-1, CE = 3.93 × 10-3 and K2/1 = 196 M-1, CE = 1.93 × 10-3 respectively. The powder X-ray diffraction results of 3DGM (βCD/DPU = 2/1, HP-βCD/DPU = 2/1) showed that the diffraction peaks originating from the DPU and βCD disappeared, indicating a halo pattern. Differential scanning calorimetry results showed an endothermic peak at 244 °C derived from the melting point of DPU, but the endothermic peak disappeared in the 3DGM (βCD/DPU = 2/1, HP-βCD/DPU = 2/1). Near-infrared absorption spectra showed peak shifts in 3DGM (βCD/DPU and HP-βCD/DPU) at the -CH and -NH groups of DPU and the -OH groups of βCDs and free water. In the dissolution test (after 5 min), the concentration of intact DPU was 0.083 μg/mL. However, the dissolution concentrations of DPU in the 3DGM (βCD/DPU = 1/1), 3DGM (βCD/DPU = 2/1), 3DGM (HP-βCD/DPU = 1/1), and 3DGM (HP-βCD/DPU = 2/1) were 3.27, 3.64, 5.70, and 7.03 μg/mL, respectively, indicating higher solubility than that of the intact DPU. Further, 1H-1H NOESY NMR spectroscopic measurements showed cross-peaks between H-A (7.32 ppm) and H-B (7.12 ppm) of DPU and H-6 (3.79 ppm) in the βCD cavity of the 3DGM (βCD/DPU = 2/1). A cross-peak was also observed among DPU H-A (7.32 ppm), H-B (7.11 ppm), and H-6 (3.78 ppm) in the βCD cavity. The results of the broccoli sprout cultivation experiment showed that 3DGM (βCD/DPU = 1/1), 3DGM (βCD/DPU = 2/1), 3DGM (HP-βCD/DPU = 1/1), and 3DGM (HP-βCD/DPU = 2/1) increased the stem thickness compared with that of the control group (DPU). These results indicated that the βCD/DPU and HP-βCD/DPU inclusion complexes were formed by the three-dimensional mixing and milling method, which enhanced the solubility and plant growth-promoting effects.

Mechanically Stimulated Solid-State Interaction of Platinum Tetrachloride with Sodium β-Diketonates.

A new mechanically stimulated solid-state reaction of PtCl4 with sodium β-diketonates has been discovered. Platinum (II) β-diketonates were obtained by grinding excess sodium trifluoroacetylacetonate Na(tfac) or hexafluoroacetylacetonate Na(hfac) in a vibration ball mill, followed by subsequent heating of the resulting mixture. The reactions occur under much milder conditions (at about 170 °C) compared to similar reactions of PtCl2 or K2PtCl6 (at about 240 °C). Excess diketonate salt plays the role of a reducing agent in the conversion of Pt (IV) salt to Pt (II) compounds. The effect of grinding on properties of the ground mixtures was studied by XRD, IR, and thermal analysis methods. The difference in the course of the interaction of PtCl4 with Na(hfac) or Na(tfac) indicates the dependence of the reaction on the ligand properties. The probable reaction mechanisms were discussed. This method of synthesis of platinum (II) β-diketonates makes it possible to substantially reduce the variety of reagents used, the number of reaction steps, the reaction time, the use of solvents, and waste generation compared to conventional solution-based methods.

Gallic acid-butyramide monohydrate cocrystal: Crystal growth, Structural insights, Theoretical calculations and Molecular docking studies against COVID-19 main protease

Single crystal X-ray diffraction is the only experimental technique available to elucidate the complete three-dimensional structure of the samples at molecular and atomic levels. But this technique demands defect-free single crystals. Growing good quality single crystals which are suitable to collect X-ray intensity data is an art rather than science. Among the various crystal growth methods, the most effective and commonly used is the slow evaporation method. Using this method, defect-free single crystals of the ground mixture of gallic acid (GA) and butyramide (BU) taken in a 1:1 molar ratio are obtained. The compound was subjected to experimental characterizations like; PXRD, FTIR, SCXRD, and TGA. Further, these results were utilized in the computational characterizations namely, Hirshfeld surface analysis, interaction energy calculations, DFT studies, and docking studies. Structural characterization revealed that the GA-BU compound was crystallized as a cocrystal hydrate with 2:1:1 stoichiometry in a monoclinic crystal system and P21/n space group. Structural studies exposed the presence of various inter and intramolecular hydrogen bond interactions, ring synthons, DDAA environment of the water molecule, and π ... π stacking interactions. The contribution of the several close contacts to the crystal structure, the influence of different interaction energies in the packing, the HOMO-LUMO energy gap, and the location of reactive sites were realized through computational studies. Further, a molecular docking study has been performed to check the antiviral activity of the title compound against COVID-19.

Pattern of Lung Involvement in Predicting Severity and Sequelae in Patients With COVID-19.

Background During the COVID pandemic, high-resolution CT scan has played a pivotal role in detecting lung involvement and severity based on the segments of the lung involved. The pattern of involvement was not considered, and our aim is to observe the pattern of lung involvement in predicting severity and guiding management protocol in patients with COVID-19. Methodology It was a prospective observational study conducted with 151 patients admitted with COVID-19with a positive reverse transcriptase polymerase chain reaction test (RT-PCR)in a single tertiary care hospital in south India. Patients with pre-existing lung pathologies were excluded from the study. Eligible patients were then divided into mild, moderate, and severe categories based on Indian Council of Medical Research (ICMR) guidelines, and high-resolution computed tomography (HRCT) chest was done, findings of which were then categorized based on lung involvement; into ground glass opacities (GGO), interstitial involvement and mixture of both. These were then analyzed to determine their importance with respect to the duration of stay and severity of the disease. Results The data collected was analyzed by IBM SPSS software version 23.0 (IBM Corp., Armonk, NY, USA). The study population included 114 males (75.5%) and 37 females (24.5%). HRCT chest was done which showed 62.3% of patients had GGO, 14.6% had interstitial lung involvement, 18.5% had a mixture of both and 4.6% had normal lung findings. These findings, when compared to clinical categories of severity, showed a significant co-relation between pattern of involvement of the lung and the severity of the disease. It also showed significant co-relation with the duration of stay. Conclusion HRCT chest has proven to be useful in the determination of patient's severity and can guide with management. We suggest earlier initiation of steroids and anticoagulants in patients with interstitial involvement even for the patients not on oxygen therapy yet. It can be used as a triage modality for screening due to the advantage of presenting with immediate results as opposed to RT-PCR which might take hours and can delay treatment which can prevent worsening.

Preparation and Spectroscopic Characterization of Inclusion Complexes of 3D Ball-Milled Rifampicin with β-cyclodextrin and γ-cyclodextrin : 3D Ball-Milled Rifampicin with β-cyclodextrin and γ-cyclodextrin.

Rifampicin (RFP) solutions, intended to reduce incidence of prosthetic graft infection, were prepared as three-dimensional ground mixtures (3DGMs) using β-cyclodextrin (βCD) and γ-cyclodextrin (γCD) and characterized for their spectroscopic properties and solubility. Phase solubility diagrams revealed that 3DGMs (RFP/βCD and RFP/γCD) produced a complex at 1:1 molar ratio. Pulsed field gradient nuclear magnetic resonance experiments indicated that the diffusion coefficients for RFP/βCD and RFP/γCD were similar to the respective diffusion coefficients for βCD and γCD. Rotating-frame Overhauser effect spectroscopy NMR spectra revealed the existence of a new exchanger peak for RFP/γCD, suggesting an intermolecular interaction different from that of RFP/βCD. Differential scanning calorimetry confirmed the presence of endothermic peak at 191°C indicating the manifestation of RFP in the inclusion complex. Interestingly, molecular interactions from the complexes, RFP/βCD and RFP/γCD, revealed different patterns of inclusion in the 3DGMs. In RFP/βCD, nuclear Overhauser effect spectroscopy NMR spectra indicated cross peaks for the protons of the methyl group of RFP and the protons (H-5 and H-6) in the βCD cavity. The methyl group of RFP interacted with the narrow rim of βCD. With RFP/γCD, cross peaks were due to the protons of the methyl group of RFP and the protons of the cavity of γCD suggesting multiple inclusion patterns. The observed multiple cross peaks affirm the inclusion of RFP into the CD cavity which enhanced its solubility by 1.6-2.0-fold when prepared as 3DGMs as RFP/βCD and RFP/γCD, respectively.

Energy-Efficient Synthetic Method, X-Ray Diffraction Analysis and Thermal Decomposition of Cobalt (II) and Nickel (II) Schiff Base Complexes Derived from 2-Aminobenzothiazole

A Schiff base was synthesized from the condensation reaction of 2-hydroxybenzaldehyde and 2-aminobenzothiazole via energy-efficient liquid-assisted mechanochemical synthesis (LAG). The Co (II) and Ni (II) complexes were also synthesized and characterized using IR, Solubility, TGA, PXRD, UV-Visible analysis, magnetic susceptibility measurement, conductivity measurement, and CHNS/O micro-analysis. In the IR analysis, the Schiff base spectrum revealed a prominent band at 1603 cm-1 (assigned to the azomethine v(C=N) stretching vibration), and the azomethine band shifted to 1621 and 1599 cm-1 in the Co (II) and Ni (II) complexes, respectively (indicating the formation of the expected complexes). In the TGA thermogram, Ni (II) and Cu (II) Schiff base complexes had decomposition temperatures of 184 and 181°C, respectively. The PXRD analysis revealed that the patterns of the ground mixture were different from the starting constituents, implying that the raw components were converted into the final product. The theoretical and experimental analytical data of C, H, and N for the Schiff base and complexes are in good agreement. The Schiff base ligand and its complexes were evaluated as agents for inhibiting the growth of pathogenic bacteria using the agar well diffusion method. According to antimicrobial activity studies, complexes exhibit stronger antibacterial activity than the Schiff base.

Preparation and Evaluation of a Powdered Rebamipide Mouthwash as In-Hospital Formulation: Considering Dispersion before Use in Patients.

In Japan, rebamipide (RB) mouthwash (RB-MW) for oral mucositis induced by cancer chemotherapy has been prepared using in-hospital formulation. Usually, RB-MW is prepared by dispersing crushed commercial RB tablets in the dispersion medium; however, uniformity is difficult to obtain due to low solubility. The current study aims is to prepare homogenously dispersed formulations using the fine particles of crushed tablets by a method that is convenient for hospital use. Commercial RB tablets were pre-milled at different milling times as “RB-Ts”. A ground mixture was then prepared by co-grinding the RB-Ts with HPC-L or PVP K30 via a benchtop ball milling machine (MM400). The physicochemical properties of samples were evaluated for PXRD, FTIR, turbidity, particle size, and solubility. Although the milling of RB tablets decreased the crystallinity, the length of milling time did not affect them. In contrast, grinding using MM400 significantly decreased RB crystallinity; their PXRD patterns showed a halo, suggesting the amorphization of RB crystals by grinding. Although solubility and turbidity seemed to be affected by the type of polymer rather than the particle size, every ground mixture showed high dispersibility. Thus, grinding the RB-Ts with polymers appeared to be the most promising way to obtain stable dispersion as an in-hospital formulation.

Low temperature in air molten synthesis of flower-like hierarchical structure SnS2 with superior photocatalysis

A molten method with the characteristics of low temperature, air environment, simplicity, cost-effectiveness and easy scale-up, was tried for the synthesis of highly photocatalytically active SnS2. By heating the ground mixture of low-melting-point S and SnCl2•2H2O powders in air at 120 °C for 6 h, phase-pure SnS2 with a nanoflake-assembled flower-like hierarchical structure was obtained. The phase, purity, microstructure, and bandgap of the obtained SnS2 (SnS2-M) were determined using a series of advanced characterization means. The photocatalytic property of SnS2-M was assessed based on the reduction of aqueous Cr(VI) with visible-light (λ > 420 nm) actuation. The photocatalytic results demonstrated that SnS2-M had extraordinarily high photocatalytic activity, which was 7 times as that of SnS2 nanoplates fabricated through hydrothermal approach. Moreover, SnS2-M showed good retention of photocatalytic performance during the recyclability tests (the Cr(VI) removal ratio was 98.9% in the first cycle and 91.6% in the third cycle).

Effect of Spatial Variability of the Elastic Modulus in Composite Ground on the Structural Performance of Large-diameter Tunnels

The spatial variability of soil properties is often neglected in design and construction, resulting in underestimating or overestimating the tunnel structural performance. Furthermore, the risks of ignoring the spatial variability of ground properties increase significantly as the tunnel diameter increases. This study investigates the effects of ground spatial variability on the convergence of shield tunnels in the composite ground, based on a real case of a cross-sea tunnel typically embedded in a ground mixture of soft clay and hard rock in Shenzhen, China. The influence of scale of fluctuation (SOF) for the soil and rock elastic modulus on tunnel convergence is investigated. It is found that the mean value of the tunnel convergence is less affected. In contrast, the tunnel convergence coefficient of variation is strongly affected by changing the elastic modulus SOF of the soil or rock layer. Moreover, the results indicate that as the elastic modulus follows the lognormal distribution, the vertical and horizontal convergence of the tunnel agrees well with the lognormal distribution.

Increasing exposure of atomically dispersed Ni sites via constructing hierarchically porous supports for enhanced electrochemical CO2 reduction

Atomically dispersed metal catalysts have been widely utilized for electrocatalysis, such as the electrochemical reduction of CO2, due to their low coordination number and maximum utilization of metal active sites. However, it remains a major challenge to develop an effective and convenient strategy for fully exposing the active sites of atomically dispersed metal catalysts within supports. Herein, we describe an operationally simple and sustainable strategy for preparing hierarchically porous thin-wall carbon networks with highly exposed atomically dispersed Ni sites by directly pyrolyzing a ground mixture of metal salts and organic ligands. Compared with the preformed metal organic framework-derived materials, the amount of exposed active Ni sites can be increased by ~50% for hierarchically porous materials. The hierarchically porous atomically dispersed Ni electrocatalyst shows obviously enhanced CO2RR catalytic performance with higher CO Faradaic efficiency (over 99% at −0.88 V) and high TOF value of 7025 h−1 (72.6% higher than that for the metal organic framework-derived materials). The excellent activity can be attributed to the increased exposure of atomically dispersed Ni sites with hierarchically porous structure and interconnected thin-wall carbon networks, which ensure the fully exposure of electrocatalytically active sites and promotion of mass transport and electron transfer. Density functional theory calculations further suggest that the fully exposed Ni sites are responsible for highly efficient activation of CO2 rather than the carbon layer-covered Ni sites.

Qualitative and quantitative analysis of mixtures of microplastics in the presence of calcium carbonate by pyrolysis-GC/MS

Environmental pollution by microplastics (MPs) has attracted much attention due to possible risks of MPs to human health, and fast and reliable analytical methods are required for identification and quantification of MPs in various matrices. Pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) has advantageous characteristics in that both identification and mass quantification can be easily done by chromatographic separation in combination with mass spectral analysis. Environmental MP samples usually contain several types of polymers and the pyrolysis of mixed polymer particles may cause a secondary reaction between pyrolyzates from different polymers. In this study, effect of the usage of calcium carbonate (CaCO3) as a catalyst on pyrolytic behavior of polymers was examined to obtain catalytic conversion of reactive pyrolyzates to stable compounds. CaCO3 was also utilized as a diluent for insoluble PE and PP powders to assure weighing easiness by forming a homogenous mixture. First, a reference material was prepared to make calibration curves by mixing twelve different types of standard polymers, selected to reflect common polymers in the global production. Identification and quantification of polymers in mixed polymer samples were validated by using model polymer mixtures, after storing Py-GC/MS data of twelve polymers with a given sample amount in a software named as F-Search MPs. Results exceeding the limit of quantitation combined with the high probability of a library match as confirmed by the software, provided assurance of the presence of the identified polymer in the model polymer mixtures. The quantitated values for the model polymer mixtures were compared with the compounded amount. The recovery varied depending on the polymer type, and especially short recovery (ca. 60–70 %) was recognized for PC in the sample from Solution A (SA) and excess recovery (ca. 175 %) for PET in the sample from Solution B (SB). Finally, the developed method was applied to the analysis of ground mixtures of isolated environmental MP particle samples and quick identification and quantification of each polymer in the MP samples were attained.

Enhanced leaching of Mo by mechanically co-grinding and activating MoS2 with NaClO3 as an oxidizing additive

The slow leaching rate of molybdenite (MoS2), due to its inert nature, and low recovery hinders the application of traditional hydrometallurgical processing. This study investigated the effects of grinding speed and time, molar ratio of sodium chlorate (NaClO3, oxidant) to MoS2, leaching time and temperature on the leaching efficiency of molybdenum (Mo). Grinding at low speeds via mechanical activation decreased particle size. However, at speeds over 450 rpm for 1.0 h, or at lower speeds but with longer time, it triggers a solid-state reaction (mechanochemistry) producing soluble Na2Mo2O7. This may be due to the existence of an energy threshold for the solid-state reaction. The most suitable activating conditions were 600 rpm for 0.5 h, with a molar ratio of NaClO3: MoS2 = 5, leached in 0.1 M NaOH solution for 2.0 h at 348 K, giving rise to a Mo recovery of 74.8%. The initial acid leaching stage of the ground mixture is dominated by the dissolution of Na2Mo2O7, giving rise to elevated Mo recovery. The later stage is controlled by the dissolution of MoS2, slowing down the increase in Mo extraction. As compared to alkaline conditions, acidic leaching of MoS2 ground at low speeds (non solid-state reaction) gives greater Mo recovery, due to the greater activity of NaClO3 to MoS2 under acidic conditions. However, the greatest Mo recovery is achieved in alkaline solution for MoS2 ground at high speed (solid-state reaction) due to the occurrence of mechanochemical reaction.

Solubility of Piperine and Its Inclusion Complexes in Biorelevant Media and Their Effect on Attenuating Mouse Ileum Contractions.

This study evaluated the solubility of piperine (PP) in biorelevant media and the effect of its ground mixtures (GMs) and coprecipitates (CPs) on intestinal contractions when presented in inclusion complexes with α-, β-, and γ-cyclodextrins (CDs). In the powder X-ray diffraction (PXRD) and differential scanning calorimetry (DSC) measurements, CP (PP/αCD) and CP (PP/γCD) suggest the formation of inclusion complexes. The 1H-nuclear magnetic resonance (NMR) analysis showed the integrated intensity ratios of CP (PP/αCD) and CP (PP/γCD) protons to be 1/2 and 1/1, the same as the respective molar ratios in the respective GM inclusion complexes. The intestinal contraction test confirmed that the intestinal contraction rate of carbachol (CCh) in the presence of 2.0 × 10–5 M PP was comparable to that in the absence of PP. On the other hand, CP (PP/αCD), GM (PP/αCD = 1/2), and GM (PP/βCD = 1/1) formed inclusion complexes that significantly suppressed the intestinal contractility at PP 1.0 × 10–8 M. No significant differences were observed between CP and GM. The solubility of the PP/αCD inclusion complex was 6–7 times higher than that of PP in the fasted-state-simulated intestinal fluid (FaSSIF, pH 6.5). PP functioned to suppress intestinal contraction by forming an inclusion complex. Based on this result, PP/αCD might be expected to be effective as an antidiarrheal.

Az önvezető autózás kihívásai és biztonsági kérdései a digitális államban

Összefoglalás. A XXI. század első felében a korábban sok évtizeden keresztül lassan változó közlekedés gyorsított ütemben alakul át. Ez alatt a pár év alatt több változás következik be, több kihívást kell leküzdeni, mint a korábbi időszakban. Az elektromos hajtás térnyerése, új járműhasználati módok mellett a járművek autonomizálódása és összekapcsolódása jelenti az új irányokat, amelyek kihívás elé állítják nemcsak az autóipart, hanem a járművek használóit és a szabályzókat, az államot is. Kutatásainkban az önvezető autózás jelentette kihívásokat emeljük ki a többi, röviden bemutatott trend közül, majd pedig vizsgáljuk, milyen kihívásokat támaszt a digitalizálódó állam felé az önvezetés felé elmozduló járműves technológia. Summary. In the first half of the 21st century, transportation that has been slowly changing over many decades has been transforming at an accelerated rate. Over the course of these few years, there will be more changes and more challenges to overcome. For a century it was unquestionable that a vehicle is driven by a driver and its energy comes via diesel or petrol from crude oil. Today vehicles’ autonomy in driving is increasing, and instead of crude oil based fuels first biocomponents and gaseous fuels appeared, and now electricity knocks at the door. The proliferation of the electric driving, the new modes of vehicle use, and the autonomy and connectivity of vehicles represent new directions that challenge not only the automotive industry, but also vehicle users and regulators, and the states. New technologies bring about new security and safety challenges as well. Most of the challenges pop up in the cyber security domain. And its result is that a closer cooperation is necessary between the automotive industry and informatics. As these two leading industrial fields have a different setup, the cooperation is energy demanding task for all participants. Modification and upgrade of the homologation process seems to be one of the potential gateways that could merge the safety requests. Improving traditionally rigid automotive homologation processes needs a lot of extended test opportunities. In our research, we highlight the challenges posed by self-driving cars and show some trends briefly, and then examine the challenges posed by vehicle technology moving towards self-driving, and towards digitizing. The certification process of the automotive industry is highlighted and modifications are proposed. We propose to extend the traditional proving ground based certification processes with special, autonomous vehicles designed processes that are partially made within the virtual reality-proving ground mixtures. A newly designed proving ground not only offers a wide range of vehicle and traffic tests for conventional, connected and automated vehicles, but can also be used to test possible prototype solutions, as well as helps to develop the type-approval process, and useful for educational purposes. Cyber security has special dimensions, newly developed test environment is necessary to validate the vehicles and their elements. A complete vehicle testing and validation center is proposed to establish for automotive cyber security features, focusing not only on known, but also on unknown vulnerabilities. It will help to develop dedicated tests to eliminate unknown vulnerabilities and potential new vulnerabilities.

Preparation and Characterization of Solid Dispersions Composed of Curcumin, Hydroxypropyl Cellulose and/or Sodium Dodecyl Sulfate by Grinding with Vibrational Ball Milling.

Solubility is an important physicochemical property affecting drug bioavailability. One approach to improve drug solubility is using amorphous formulations, which can improve solubility by up to a 1000-fold. Herein, amorphous curcumin (CUR) and amorphous solid dispersions (SDs) consisting of CUR, hydroxypropyl cellulose (HPC) and/or sodium dodecyl sulfate (SDS) were developed using vibrational ball milling. The resulting ground mixtures (GMs) were characterized using powder X-ray diffractometry, Fourier transform infrared spectroscopy, differential scanning calorimetry and a dissolution test. The 60-min GM containing 90% HPC significantly increased the drug solubility. Presence of SDS in the GMs containing 90% HPC reduced the grinding duration from 60 min to 30 min in forming a ground SD that significantly increased the CUR dissolution rate. This amorphous state was stable for 30 days when stored at 40 °C/RH 75%.

Enhancing the Solubility of Curcumin Using a Solid Dispersion System with Hydroxypropyl-β-Cyclodextrin Prepared by Grinding, Freeze-Drying, and Common Solvent Evaporation Methods.

Cyclodextrins (CDs) and their derivatives significantly increase drug solubility by forming drug/CD complexes known as solid dispersions (SDs), which consist of an inclusion complex (IC), where the drug is entrapped within the CD cavity, and a non-IC. Here, the SDs of curcumin (CUR) and hydroxypropyl-β-cyclodextrin (HPβCD) were prepared using the grinding, freeze-drying (FD), and common solvent evaporation (CSE) methods and were physicochemically characterized using solubility, powder X-ray diffraction, Fourier transform infrared, differential scanning calorimetry, and dissolution studies. The second or higher order complex of CUR-HPβCD indicated the co-existence of ICs and non-ICs known as the SD system. When comparing the soluble drug amount with CUR crystals, the solubility of SDs was enhanced by up to 299-, 180-, and 489-fold, corresponding to the ground mixtures (GMs), freeze-drying mixtures (FDs), and common solvent evaporation mixtures (CSEs), respectively. The total transformation into the amorphous phase of CUR was observed in GMs and in CSE12, CSE14, and CSE18. The drug was well dispersed within HPβCD in GMs and CSEs, suggesting the formation of hydrogen bonds between CUR and HPβCD, whereas the dispersed behavior of FDs was similar to that of physical mixtures. In SDs, the melting temperature of CUR was in an increased order of CUR in 1:2 ICs, CUR in 1:1 ICs, and CUR crystals. The dissolution rate of CUR was positively improved as the amount of HPβCD in SDs increased. The SD system consisting of CUR and HPβCD significantly increased the drug solubility compared to ICs.

Preparation and Evaluation of Rebamipide Colloidal Nanoparticles Obtained by Cogrinding in Ternary Ground Mixtures

Aphthous stomatitis is one of the side effects of chemotherapy and radiotherapy in cancer treatment. Rebamipide (RB) mouthwash for stomatitis acts as a radical scavenger. However, RB is poorly soluble in water, which leads to aggregation and precipitation of the dispersoid. The particle size of the drug needs to be less than 100 nm for the particles to reach the mucus layer in the oral cavity. In this study, we attempted to prepare nanoparticles of RB by cogrinding with polyvinylpyrrolidone (PVP) or hydroxypropyl cellulose (HPC) and sodium dodecyl sulfate (SDS) using a mixer ball mill, and evaluated the physicochemical properties of RB nanoparticles, the stability of dispersion in water, and permeation of the mucus layer in vitro. By cogrinding, the particle size decreased to around 110 nm, and powder X-ray diffraction (PXRD) of the particles showed totally broad halo patterns, which suggested a decreased crystalline region. Furthermore, the solubility of RB nanoparticles increased by approximately fourfold compared with RB crystals, and the water dispersibility and permeation of the mucus layer were improved. The results suggest that in a ternary ground mixture of RB, PVP or HPC, and SDS, the RB nanoparticles obtained can be applied as a formulation for stomatitis.