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1.
Int J Mol Sci ; 25(7)2024 Mar 22.
Artículo en Inglés | MEDLINE | ID: mdl-38612389

RESUMEN

Alkaline earth metal oxide (MgO, CaO, SrO) catalysts supported on BEA zeolite were prepared by a wet impregnation method and tested in the transesterification reaction of rapeseed oil with methanol towards the formation of biodiesel (FAMEs-fatty acid methyl esters). To assess the influence of the SiO2/Al2O3 ratio on the catalytic activity in the tested reaction, a BEA zeolite carrier material with different Si/Al ratios was used. The prepared catalysts were tested in the transesterification reaction at temperatures of 180 °C and 220 °C using a molar ratio of methanol/oil reagents of 9:1. The transesterification process was carried out for 2 h with the catalyst mass of 0.5 g. The oil conversion value and efficiency towards FAME formation were determined using the HPLC technique. The physicochemical properties of the catalysts were determined using the following research techniques: CO2-TPD, XRD, BET, FTIR, and SEM-EDS. The results of the catalytic activity showed that higher activity in the tested process was confirmed for the catalysts supported on the BEA zeolite characterized by the highest silica/alumina ratio for the reaction carried out at a temperature of 220 °C. The most active zeolite catalyst was the 10% CaO/BEA system (Si/Al = 300), which showed the highest triglyceride (TG) conversion of 90.5% and the second highest FAME yield of 94.6% in the transesterification reaction carried out at 220 °C. The high activity of this system is associated with its alkalinity, high value of the specific surface area, the size of the active phase crystallites, and its characteristic sorption properties in relation to methanol.


Asunto(s)
Biocombustibles , Zeolitas , Óxido de Magnesio , Metanol , Aceite de Brassica napus , Dióxido de Silicio , Ácidos Grasos , Óxidos
2.
Molecules ; 29(12)2024 Jun 16.
Artículo en Inglés | MEDLINE | ID: mdl-38930922

RESUMEN

The impact of heterogeneous catalytic systems, which are based on rare earth metals, on the properties of biodiesel produced via the transesterification process in a stationary reactor (autoclave) was thoroughly investigated. The physicochemical attributes, including the specific surface area, were analyzed employing the Brunauer-Emmett-Teller (BET) method. The basicity and acidity levels of the catalytic systems were evaluated through temperature-programmed desorption of ammonia and carbon dioxide (TPD-NH3, TPD-CO2), respectively. Furthermore, High-Performance Liquid Chromatography (HPLC) analysis facilitated the assessment of triglyceride conversion and the determination of methyl ester (FAME) selectivity within these processes. Our findings indicate that catalytic systems augmented with lanthanum showcased superior performance. A significant correlation was discerned between the conversion and selectivity to methyl esters and both the specific surface area and the acidity and basicity properties of the catalytic systems under study. These results underscore the crucial role that the physicochemical characteristics of catalytic systems play in optimizing the transesterification process, thereby enhancing the quality of the produced biodiesel. This study contributes valuable insights into the development of more efficient and effective biodiesel production methodologies, highlighting the potential of rare earth metal-based catalysts in renewable energy technologies.

3.
Molecules ; 29(7)2024 Mar 22.
Artículo en Inglés | MEDLINE | ID: mdl-38611697

RESUMEN

This work is focused on the application of lanthanide-free perovskite Ba1-xSrxTiO3 (0 < x < 1) in valorization of toxic pollutants as 4-nitrophenol (4-NPh). The series of perovskites were fabricated by facile, one-step solid-state preparation method and characterized via various techniques: elemental analysis (Inductively Coupled Plasma Optical Emission Spectrometry, ICP-OES), powder X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR) and dielectric properties (impedance spectroscopy, IS). The methods confirmed the assumed composition, structure and high purity of the materials. The results showed that substitution of Ba2+ by Sr2+ in the perovskite crystal lattice influenced the dielectric properties of samples and the size of the grains. The absorption and catalytic properties of Ba(1-x)SrxTiO3 (0 < x < 1) series were evaluated in reduction of 4-NPh in water using NaBH4 as reducing agent. No adsorption of 4-NPh was found for all the materials during 180 min of contact (experiment without reducing agent), and the best catalytic performance was found for the Ba(1-x)SrxTiO3 (x = 0.3) sample. The catalytic transformation of 4-NPh to 4-APh follows a pseudo-first-order model, and the catalysts can be easily regenerated via mild annealing (300 °C).

4.
Int J Mol Sci ; 24(1)2023 Jan 01.
Artículo en Inglés | MEDLINE | ID: mdl-36614204

RESUMEN

The three Schiff base ligands, derivatives of hesperetin, HHSB (N-[2,3-dihydro-5,7-dihydroxy-2-(3-hydroxy-4-methoxyphenyl)chromen-4-ylidene]isonicotinohydrazide), HIN (N-[2,3-dihydro-5,7-dihydroxy-2-(3-hydroxy-4-methoxyphenyl)chromen-4-ylidene]benzhydrazide) and HTSC (N-[2,3-dihydro-5,7-dihydroxy-2-(3-hydroxy-4-methoxyphenyl)chromen-4-ylidene]thiosemicarbazide) and their copper complexes, CuHHSB, CuHIN, and CuHTSC were designed, synthesized and analyzed in terms of their spectral characterization and the genotoxic activity. Their structures were established using several methods: elemental analysis, FT-IR, UV-Vis, EPR, and ESI-MS. Spectral data showed that in the acetate complexes the tested Schiff bases act as neutral tridentate ligand coordinating to the copper ion through two oxygen (or oxygen and sulphur) donor atoms and a nitrogen donor atom. EPR measurements indicate that in solution the complexes keep their structures with the ligands remaining bound to copper(II) in a tridentate fashion with (O-, N, Oket) or (O-, N, S) donor set. The genotoxic activity of the compounds was tested against model tumour (HeLa and Caco-2) and normal (LLC-PK1) cell lines. In HeLa cells the genotoxicity for all tested compounds was noticed, for HHSB and CuHHSB was the highest, for HTSC and CuHTSC-the lowest. Generally, Cu complexes displayed lower genotoxicity to HeLa cells than ligands. In the case of Caco-2 cell line HHSB and HTSC induced the strongest breaks to DNA. On the other side, CuHHSB and CuHTSC induced the highest DNA damage against LLC-PK1.


Asunto(s)
Complejos de Coordinación , Cobre , Humanos , Cobre/farmacología , Cobre/química , Bases de Schiff/farmacología , Bases de Schiff/química , Espectroscopía Infrarroja por Transformada de Fourier , Células HeLa , Células CACO-2 , Oxígeno , Complejos de Coordinación/farmacología , Complejos de Coordinación/química , Ligandos
5.
Molecules ; 28(19)2023 Sep 30.
Artículo en Inglés | MEDLINE | ID: mdl-37836736

RESUMEN

The encapsulation of insoluble compounds can help improve their solubility and activity. The effects of cyclodextrin encapsulation on hesperetin's derivatives (HHSB, HIN, and HTSC) and the physicochemical properties of the formed complexes were determined using various analytical techniques. The antioxidant (DPPH•, ABTS•+ scavenging, and Fe2+-chelating ability), cytotoxic, and antibacterial activities were also investigated. The inclusion systems were prepared using mechanical and co-evaporation methods using a molar ratio compound: HP-ß-CD = 1:1. The identification of solid systems confirmed the formation of two inclusion complexes at hesperetin (CV) and HHSB (mech). The identification of systems of hesperetin and its derivatives with HP-ß-CD in solutions at pHs 3.6, 6.5, and 8.5 and at various temperatures (25, 37 and 60 °C) confirmed the effect of cyclodextrin on their solubility. In the DPPH• and ABTS•+ assay, pure compounds were characterized by higher antioxidant activity than the complexes. In the FRAP study, all hesperetin and HHSB complexes and HTSC-HP-ß-CD (mech) were characterized by higher values of antioxidant activity than pure compounds. The results obtained from cytotoxic activity tests show that for most of the systems tested, cytotoxicity increased with the concentration of the chemical, with the exception of HP-ß-CD. All systems inhibited Escherichia coli and Staphylococcus aureus.


Asunto(s)
Antioxidantes , Ciclodextrinas , 2-Hidroxipropil-beta-Ciclodextrina/química , Antioxidantes/farmacología , Antioxidantes/química , Ciclodextrinas/farmacología , Ciclodextrinas/química , Solubilidad
7.
Int J Mol Sci ; 22(16)2021 Aug 23.
Artículo en Inglés | MEDLINE | ID: mdl-34445779

RESUMEN

This work interrogates for the first time the catalytic properties of various monometallic Ni catalysts in the oxy-steam reforming of LNG. Various research techniques, including X-ray diffraction (XRD), specific surface area and porosity analysis (BET method), scanning electron microscopy with X-ray microanalysis (SEM-EDS), temperature-programmed desorption of ammonia (TPD-NH3), temperature-programmed reduction (TPR-H2) and the FTIR method, were used to study their physicochemical properties. The mechanism of the oxy-steam reforming of LNG is also discussed in this paper. The high activity of monometallic catalysts supported on 5% La2O3-CeO2 and 5% ZrO2-CeO2 oxides in the studied process have been proven and explained on the basis of their acidity, specific surface area, sorption properties in relation to the reaction products, the crystallite size of the metallic nickel and their phase composition.


Asunto(s)
Cerio/química , Lantano/química , Níquel/química , Óxidos/química , Óxido de Aluminio/química , Amoníaco/química , Catálisis , Hidrógeno/química , Gas Natural , Vapor , Temperatura , Difracción de Rayos X/métodos
8.
Int J Mol Sci ; 22(10)2021 05 19.
Artículo en Inglés | MEDLINE | ID: mdl-34069455

RESUMEN

In this work, we report solvent-induced complexation properties of a new N2S2 tetradentate bis-thiosemicarbazone ligand (H2LI), prepared by the condensation of 4-phenylthiosemicarbazide with bis-aldehyde, namely 2,2'-(ethane-1,2-diylbis(oxy)dibenzaldehyde, towards nickel(II). Using ethanol as a reaction medium allowed the isolation of a discrete mononuclear homoleptic complex [NiLI] (1), for which its crystal structure contains three independent molecules, namely 1-I, 1-II, and 1-III, in the asymmetric unit. The doubly deprotonated ligand LI in the structure of 1 is coordinated in a cis-manner through the azomethine nitrogen atoms and the thiocarbonyl sulfur atoms. The coordination geometry around metal centers in all the three crystallographically independent molecules of 1 is best described as the seesaw structure. Interestingly, using methanol as a reaction medium in the same synthesis allowed for the isolation of a discrete mononuclear homoleptic complex [Ni(LII)2] (2), where LII is a monodeprotonated ligand 2-(2-(2-(2-(dimethoxymethyl)phenoxy)ethoxy)benzylidene)-N-phenylhydrazine-1-carbothioamide (HLII). The ligand LII was formed in situ from the reaction of LI with methanol upon coordination to the metal center under synthetic conditions. In the structure of 2, two ligands LII are coordinated in a trans-manner through the azomethine nitrogen atom and the thiocarbonyl sulfur atom, also yielding a seesaw coordination geometry around the metal center. The charge and energy decomposition scheme ETS-NOCV allows for the conclusion that both structures are stabilized by a bunch of London dispersion-driven intermolecular interactions, including predominantly N-H∙∙∙S and N-H∙∙∙O hydrogen bonds in 1 and 2, respectively; they are further augmented by less typical C-H∙∙∙X (where X = S, N, O, π), CH∙∙∙HC, π∙∙∙π stacking and the most striking, attractive long-range intermolecular C-H∙∙∙Ni preagostic interactions. The latter are found to be determined by both stabilizing Coulomb forces and an exchange-correlation contribution as revealed by the IQA energy decomposition scheme. Interestingly, the analogous long-range C-H∙∙∙S interactions are characterized by a repulsive Coulomb contribution and the prevailing attractive exchange-correlation constituent. The electron density of the delocalized bonds (EDDB) method shows that the nickel(II) atom shares only ~0.8|e| due to the σ-conjugation with the adjacent in-plane atoms, demonstrating a very weak σ-metalloaromatic character.


Asunto(s)
Níquel/química , Tiosemicarbazonas/química , Aldehídos/química , Compuestos Azo/química , Complejos de Coordinación/química , Cristalografía por Rayos X/métodos , Enlace de Hidrógeno , Ligandos , Modelos Moleculares , Estructura Molecular , Solventes/química , Tiosemicarbazonas/metabolismo
9.
Beilstein J Org Chem ; 16: 1436-1446, 2020.
Artículo en Inglés | MEDLINE | ID: mdl-32647545

RESUMEN

The McKenna reaction is a well-known and popular method for the efficient and mild synthesis of organophosphorus acids. Bromotrimethylsilane (BTMS) is the main reagent in this reaction, which transforms dialkyl phosphonate esters into bis(trimethylsilyl)esters, which are then easily converted into the target acids. However, the versatile character of the McKenna reaction is not always used to its full extent, due to formation of side products. Herein, demonstrated by using model examples we have not only analyzed the typical side processes accompanying the McKenna reaction, but also uncovered new ones. Further, we discovered that some commonly recommended precautions did not always circumvent the side reactions. The proposed results and recommendations may facilitate the synthesis of phosphonic acids.

10.
Molecules ; 24(5)2019 Mar 01.
Artículo en Inglés | MEDLINE | ID: mdl-30832297

RESUMEN

In this study, novel organic⁻inorganic composites were prepared by the complexation of dicarboxylic azo dye (AD) with aluminum⁻magnesium hydroxycarbonate (AlMg⁻LH). This procedure provides an effective method for the stabilization of dicarboxylic organic chromophores on an AlMg-LH host. The structures of the hybrid composites were examined by X-ray diffraction (XRD), secondary ion mass spectrometry (TOF-SIMS), 27-Al solid-state nuclear magnetic resonance (NMR) spectroscopy, thermogravimetric analysis (TGA) and scanning transmission electron microscopy (STEM). The TOF-SIMS method was applied to investigate the metal⁻dye interactions and to monitor the thermal stability of the organic⁻inorganic complexes. Secondary ion mass spectrometry confirmed the presence of a characteristic peak for C18H10O5N2Mg22+, indicating that both carboxylic groups interacted with AlMg-LH by forming complexes with two Mg2+ ions. Modification with hybrid pigments affected the crystal structure of the AlMg-LH mineral, as shown by the appearance of new peaks on the X-ray diffraction patterns. Adsorption of the dicarboxylic chromophore not only led to significantly enhanced solvent resistance but also improved the thermal and photostability of the hybrid pigments. We propose a possible arrangement of the azo dye in the inorganic matrix, as well as the presumed mechanism of stabilization.


Asunto(s)
Hidróxido de Aluminio/química , Compuestos Azo/química , Carbonatos/química , Compuestos Inorgánicos/química , Hidróxido de Magnesio/química , Compuestos Orgánicos/química , Hidróxido de Aluminio/síntesis química , Compuestos Azo/síntesis química , Carbonatos/síntesis química , Compuestos Inorgánicos/síntesis química , Hidróxido de Magnesio/síntesis química , Espectroscopía de Resonancia Magnética , Microscopía Electrónica de Rastreo , Compuestos Orgánicos/síntesis química , Termogravimetría , Difracción de Rayos X
11.
Molecules ; 24(3)2019 Feb 03.
Artículo en Inglés | MEDLINE | ID: mdl-30717480

RESUMEN

In this study, hybrid pigments based on carminic acid (CA) were synthesized and applied in polymer materials. Modification of aluminum-magnesium hydroxycarbonate (LH) with CA transformed the soluble chromophore into an organic-inorganic hybrid colorant. Secondary ion mass spectroscopy (TOF-SIMS), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and UV-Vis spectroscopy were used to study the structure, composition, and morphology of the insoluble LH/CA colorant. Successful modification of the LH was confirmed by the presence of interactions between the LH matrix and molecules of CA. XPS analysis corroborated the presence of CA complexes with Mg2+ ions in the LH host. The batochromic shift in UV-Vis spectra of the organic-inorganic hybrid colorant was attributed to metal-dye interactions in the organic-inorganic hybrid colorants. Strong metal-dye interactions may also be responsible for the improved solvent resistance and chromostability of the modified LH. In comparison to uncolored ethylene-norbornene copolymer (EN), a modified EN sample containing LH/CA pigment showed lower heat release rate (HRR) and reduced total heat release (THR), providing the material with enhanced flame retardancy.


Asunto(s)
Hidróxido de Aluminio/química , Carbonatos/química , Carmín/química , Hidróxido de Magnesio/química , Polímeros/química , Estructura Molecular , Espectroscopía de Fotoelectrones , Pigmentos Biológicos/química , Termogravimetría , Difracción de Rayos X
12.
Acta Crystallogr C ; 69(Pt 7): 781-6, 2013 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-23832043

RESUMEN

The crystal structures of three new solvates of olanzapine [systematic name: 2-methyl-4-(4-methylpiperazin-1-yl)-10H-thieno[2,3-b][1,5]benzodiazepine], namely olanzapine acetic acid monosolvate, C17H20N4S·C2H4O2, (I), olanzapine propan-2-ol hemisolvate monohydrate, C17H20N4S·0.5C3H8O·H2O, (II), and olanzapine propan-2-one hemisolvate monohydrate, C17H20N4S·0.5C3H6O·H2O, (III), are presented and compared with other known olanzapine forms. There is a fairly close resemblance of the molecular conformation for all studied analogues. The crystal structures are built up through olanzapine dimers, which are characterized via C-H...π interactions between the aliphatic fragment (1-methylpiperazin-4-yl) and the aromatic fragment (benzene system). All solvent (guest) molecules participate in hydrogen-bonding networks. The crystal packing is sustained via intermolecular N(host)-H···O(guest), O(guest)-H···N(host), O(guest)-H···O(guest) and C(host)-H···O(guest) hydrogen bonds. It should be noted that the solvent propan-2-ol in (II) and propan-2-one in (III) show orientational disorder. The propan-2-ol molecule lies close to a twofold axis, while the propan-2-one molecule resides strictly on a twofold axis through the carbonyl C atom. In both cases, the water molecules present positional disorder of the H atoms.


Asunto(s)
Ácido Acético/química , Benzodiazepinas/química , Piperazinas/química , Propanoles/química , Acetona/análogos & derivados , Cristalografía por Rayos X , Enlace de Hidrógeno , Estructura Molecular , Olanzapina
13.
Acta Crystallogr C ; 69(Pt 6): 630-3, 2013 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-23744384

RESUMEN

Low-temperature X-ray diffraction experiments were employed to investigate the crystal structures of an orthorhombic polymorph of the intramolecular cyclization product of perindopril, a popular angiotensive-converting enzyme (ACE) inhibitor, namely ethyl (2S)-2-[(3S,5aS,9aS,10aS)-3-methyl-1,4-dioxo-5a,6,7,8,9,9a,10,10a-octahydro-3H-pyrazino[1,2-a]indol-2-yl]pentanoate, C19H30N2O4, (Io), and its tetragonal equivalent, (It), which was previously reported at ambient temperature [Bojarska et al. (2013). J. Chil. Chem. Soc. 58, 1415-1417]. Polymorph (Io) crystallizes in the orthorhombic space group P2(1)2(1)2(1) with two molecules in the asymmetric unit, while tetragonal form (It) crystallizes in the space group P4(1)2(1)2 with one molecule in the asymmetric unit. The geometric parameters of (Io) are very similar to those of (It). The six-membered rings in both polymorphs adopt a slightly deformed chair conformation and the piperazinedione rings are in a boat conformation. However, the proline rings adopt an envelope conformation in (Io), while in (It) the ring exists in a slightly deformed half-chair conformation. The most significant difference between the two structures is the orientation of the ethyl pentanoate chain. Molecules associate in pairs in a head-to-tail manner forming infinite columns. In (Io), molecules are related by a twofold screw axis forming identical columns, while in (It), molecules in successive neighbouring columns are related by alternating twofold screw axes and fourfold screw axes. In both cases, the crystal packing is stabilized by weak intermolecular C-H···O interactions only.


Asunto(s)
Perindopril/química , Cristalización , Cristalografía por Rayos X , Ciclización , Modelos Moleculares , Conformación Molecular
14.
Materials (Basel) ; 16(3)2023 Jan 31.
Artículo en Inglés | MEDLINE | ID: mdl-36770219

RESUMEN

The main goal of this study was to modify the activity of Pd/TiO2/Ti catalyst in the reaction of CO oxidation by the addition of Zn. Plasma electrolytic oxidation (PEO) of Ti wire was conducted to produce a uniform porous layer of TiO2. A mixture of Pd and Zn was then introduced by means of adsorption. After reduction treatment, the activity of the samples was examined by oxidation of 5% CO in a temperature range from 80-350 °C. Model catalysts with sufficient amounts of the metals for physico-chemical investigation were prepared to further investigate the reaction between Pd and Zn during CO oxidation. The structures and compositions of the samples were investigated using scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS), time-of-flight secondary ion mass spectrometry (TOF-SIMS), inductively coupled plasma mass spectrometry (ICP-MS), Fourier transform infrared (FTIR), and X-ray diffraction (XRD). Modification of Pd/TiO2/Ti catalyst by Zn with a Pd:Zn atomic ratio of 2:1 decreased the temperature of complete CO oxidation from 220 °C for Pd/TiO2/Ti to 180 °C for Pd-Zn/TiO2/Ti. The temperature of 50% CO conversion on Pd-Zn(2:1)/TiO2/Ti was around 55 °C lower than in the reaction on monometallic Pd catalyst. The addition of Zn to the Pd catalyst lowered the binding energy of CO on the surface and improved the dissociative adsorption of oxygen, facilitating the oxidation of CO. FTIR showed that the bridging form of adsorbed CO is preferred on bimetallic systems. Analysis of the surface compositions of the samples (SEM-EDS, TOF-SIMS) showed higher amounts of oxygen on the bimetallic systems.

15.
Materials (Basel) ; 16(8)2023 Apr 18.
Artículo en Inglés | MEDLINE | ID: mdl-37110015

RESUMEN

The investigation of the course of the Boudouard reaction and methane cracking was performed over nickel catalysts based on oxides of calcium, aluminum, and magnesium. The catalytic samples were synthesized by the impregnation method. The physicochemical characteristics of the catalysts were determined using atomic adsorption spectroscopy (AAS), Brunauer-Emmett-Teller method analysis (BET), temperature-programmed desorption of ammonia and carbon dioxide (NH3- and CO2-TPD), and temperature-programmed reduction (TPR). Qualitative and quantitative identification of formed carbon deposits after the processes were carried out using total organic carbon analysis (TOC), temperature-programmed oxidation (TPO), X-ray diffraction (XRD), and scanning electron microscopy (SEM). The selected temperatures for the Boudouard reaction and methane cracking (450 and 700 °C, respectively) were found to be optimal for the successful formation of graphite-like carbon species over these catalysts. It was revealed that the activity of catalytic systems during each reaction is directly related to the number of weakly interacted nickel particles with catalyst support. Results of the given research provide insight into the mechanism of carbon deposit formation and the role of the catalyst support in this process, as well as the mechanism of the Boudouard reaction.

16.
Acta Crystallogr C ; 68(Pt 9): o341-3, 2012 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-22935500

RESUMEN

The dimethyl sulfoxide hemisolvate of perindoprilat [systematic name: (1S)-2-((S)-{1-[(2S,3aS,7aS)-2-carboxyoctahydro-1H-indol-1-yl]-1-oxopropan-2-yl}azaniumyl)pentanoate dimethyl sulfoxide hemisolvate], C(17)H(28)N(2)O(5)·0.5C(2)H(6)OS, an active metabolite of perindopril, has been synthesized, structurally characterized by single-crystal X-ray diffraction and compared with its ethanol disolvate analogue [Pascard et al. (1991). J. Med. Chem. 34, 663-669]. Both compounds crystallize in the orthorhombic P2(1)2(1)2(1) space group in the same zwitterionic form, with a protonated alanine N atom and an anionic carboxylate group at the n-alkyl chain. The three structural units present in the unit cell (two zwitterions and the solvent molecule) are held together by a rich system of O-H···O, N-H···O and C-H···O hydrogen-bond contacts.


Asunto(s)
Aniones/química , Indoles/química , Cristalización , Cristalografía por Rayos X , Enlace de Hidrógeno , Estructura Molecular , Solventes/química , Estereoisomerismo
17.
Acta Crystallogr C ; 68(Pt 11): o443-6, 2012 Nov.
Artículo en Inglés | MEDLINE | ID: mdl-23124459

RESUMEN

The title compound [systematic name: (1S)-2-((S)-{1-[(2S,3aS,7aS)-2-carboxyoctahydro-1H-indol-1-yl]-1-oxopropan-2-yl}azaniumyl)pentanoate monohydrate], C(17)H(28)N(2)O(5)·H(2)O, (I)·H(2)O, the active metabolite of the antihypertensive and cardiovascular drug perindopril, was obtained during polymorphism screening of perindoprilat. It crystallizes in the chiral orthorhombic space group P2(1)2(1)2(1), the same as the previously reported ethanol disolvate [Pascard, Guilhem, Vincent, Remond, Portevin & Laubie (1991). J. Med. Chem. 34, 663-669] and dimethyl sulfoxide hemisolvate [Bojarska, Maniukiewicz, Sieron, Fruzinski, Kopczacki, Walczynski & Remko (2012). Acta Cryst. C68, o341-o343]. The asymmetric unit of (I)·H(2)O contains one independent perindoprilat zwitterion and one water molecule. These interact via strong hydrogen bonds to give a cyclic R(2)(2)(7) synthon, which provides a rigid molecular conformation. The geometric parameters of all three forms are similar. The conformations of the perhydroindole group are almost identical, but the n-alkyl chain has conformational freedom. A three-dimensional hydrogen-bonding network of O-H···O and N-H···O interactions is observed in the crystal structure of (I)·H(2)O, similar to the other two solvates, but because of the presence of different solvents the three crystal structures have diverse packing motifs. All three solvatomorphs are additionally stabilized by nonclassical weak C-H···O contacts.


Asunto(s)
Dimetilsulfóxido/química , Indoles/química , Cristalografía por Rayos X , Enlace de Hidrógeno , Estructura Molecular
18.
Polymers (Basel) ; 13(24)2021 Dec 19.
Artículo en Inglés | MEDLINE | ID: mdl-34961006

RESUMEN

A new strain of bacteria producing cellulose was isolated from Kombucha and identified as Komagataeibacter hansenii, named SI1. In static conditions, the strain synthesises bacterial nanocellulose with an improved ability to stretch. In this study, utilisation of various carbon and nitrogen sources and the impact of initial pH was assessed in terms of bacterial nanocellulose yield and properties. K. hansenii SI1 produces cellulose efficiently in glycerol medium at pH 5.0-6.0 with a yield of 3.20-3.60 g/L. Glucose medium led to the synthesis of membrane characterised by a strain of 77%, which is a higher value than in the case of another Komagataeibacter species. Supplementation of medium with vitamin C results in an enhanced porosity and improves the ability of bacterial nanocellulose to stretch (up to 123%). The properties of modified membranes were studied by scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction and mechanical tests. The results show that bacterial nanocellulose produced in SH medium and vitamin C-supplemented medium has unique properties (porosity, tensile strength and strain) without changing the chemical composition of cellulose. The method of production BNC with altered properties was the issue of Polish patent application no. P.431265.

19.
Int J Biol Macromol ; 187: 584-593, 2021 Sep 30.
Artículo en Inglés | MEDLINE | ID: mdl-34324907

RESUMEN

This study aims to examine the effect of ethanol and lactic acid on the production of bacterial cellulose, and determine the optimal composition of a co-supplemented culture using response surface methodology. Both ethanol and lactic acid, when added separately or jointly, affected the yield and properties of the biomaterial. Optimization resulted in an increase of 470% in the yield, compared to the Schramm-Hestrin medium. Culture growth profiles, substrate consumption and by-products generation, were examined. The growth rate was increased for cultures supplemented with lactic acid and both lactic acid and ethanol, while the production of gluconic acid was diminished for all modified cultures. The properties of BNC, such as the structure, crystallinity, water holding capacity and tensile strength, were also determined. BNC produced in optimal conditions is more porous and characterized by wider fibers. Despite a decrease in crystallinity, by the addition of ethanol, lactic acid and both additives, the ratio of cellulose Iα was almost unchanged. The stress, strain, young modulus and toughness were improved 2.8-4.2 times, 1-1.9 times, 2.4-3.5 times and 2.5-6.8 times, respectively. The new approach to improving BNC yields and properties presented here could contribute to more economical production and wider application of this biopolymer.


Asunto(s)
Celulosa/biosíntesis , Etanol/farmacología , Gluconacetobacter xylinus/efectos de los fármacos , Ácido Láctico/farmacología , Ácido Acético/metabolismo , Celulosa/química , Cristalización , Módulo de Elasticidad , Gluconacetobacter xylinus/crecimiento & desarrollo , Gluconacetobacter xylinus/metabolismo , Gluconatos/metabolismo , Glucosa/metabolismo , Concentración de Iones de Hidrógeno , Resistencia a la Tracción , Agua/química
20.
J Funct Biomater ; 12(2)2021 May 20.
Artículo en Inglés | MEDLINE | ID: mdl-34065271

RESUMEN

Recently, the modification of the initial structure of biopolymers, mainly chitosan, has been gaining importance with a view to obtain functional forms with increased practicality and specific properties enabling their use in tissue engineering. Therefore, in this article, the properties (structural and biological) of thermosensitive hydrogels obtained from chitosan lactate/chloride and two types of crosslinking agents (ß-glycerol phosphate disodium salt pentahydrate and uridine 5'-monophosphate disodium salt) are discussed. The aim of the research is to identify changes in the structure of the biomaterials during conditioning in water. Structural investigations were carried out by FTIR spectroscopy. The crystallinity of gels was determined by X-ray diffraction analysis. The biocompatibility (evaluation of cytotoxicity and genotoxicity) of chitosan hydrogels was investigated by contact with human colon adenocarcinoma cell line for 48 h. The cytotoxicity was verified based on the colorimetric resazurin assay, and the genotoxicity was checked by the comet assay (percentage of DNA in the comet tail). The conducted research showed that the analyzed types of chitosan hydrogels are non-cytotoxic and non-genotoxic materials. The good biocompatibility of chitosan hydrogels surfaces makes them interesting scaffolds with clinical potential in tissue regeneration engineering.

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