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1.
Environ Sci Technol ; 2024 Feb 06.
Article in English | MEDLINE | ID: mdl-38319840

ABSTRACT

The design of efficient catalysts for catalytic ethylene (C2H4) oxidation is of crucial importance for extending the shelf life of fruits and vegetables. Herein, a carbon modified SBA-15 supported Pt catalyst (Pt/CSBA-15) was prepared in situ by a facile solid phase grinding-infiltration-inert atmosphere calcination method. Characterization results reveal that in the Pt/CSBA-15 catalysts thin carbon layers are successfully formed in the hexagonal pores of SBA-15. Additionally, Pt particles are well dispersed in the channels of SBA-15, and Pt/CSBA-15 has a smaller Pt particle size than the catalyst without carbon modification (i.e., Pt/SBA-15). O2 is more feasibly adsorbed and activated on small-sized Pt particles, and in situ formed carbon species enhance the hydrophobicity of catalysts. As a result, both 3Pt/CSBA-15 and 5Pt/CSBA-15 are able to maintain 100% conversion of 50 ppm of C2H4 for more than 7 h at 0 °C. 3Pt/CSBA-15 even achieves 81.5% C2H4 conversion and 71.6% CO2 yield after 20 h, exhibiting much more prominent catalytic performances than 3Pt/SBA-15. DFT calculations and in situ FTIR measurements confirm that small-sized Pt particles possess strong O2 affinity to promote O2 adsorption, and in situ formed hydrophobic carbon layers efficiently suppress competitive H2O adsorption. Such a unique one-step catalyst preparation method for regulating the size of metal particles and the hydrophobicity of catalysts can be perfectly utilized to develop simple and efficient hydrophobic catalysts applied in low-temperature oxidation of C2H4.

2.
Int J Mol Sci ; 25(2)2024 Jan 16.
Article in English | MEDLINE | ID: mdl-38256167

ABSTRACT

A new mononuclear Cu(II) complex [Cu(L2)(H2O)2], where L is the Schiff base 2-[2-(3-bromopropoxy)benzylideneamino] benzoic acid, was synthesized and covalently anchored onto an amino-functionalized SBA-15 mesoporous silica in order to obtain an efficient heterogeneous catalyst. The elemental, structural, textural and morphological characterization confirmed the coordination of the central Cu(II) ion with two ligands and two H2O molecules in the synthesized complex and its successful immobilization into the inner pore surface of the NH2-functionalized support without the loss of the mesoporous structure. The catalytic activity of the free or immobilized Cu(II) complex was tested in the oxidation of cyclohexene with H2O2 under an air atmosphere and the dismutation reaction of the superoxide radical anions with very good results. In addition, catalyst reuse tests claim its suitability in alkene oxidation processes or as a biomimetic catalyst.


Subject(s)
Biomimetics , Copper , Hydrogen Peroxide , Schiff Bases , Silicon Dioxide
3.
Int J Mol Sci ; 25(7)2024 Apr 03.
Article in English | MEDLINE | ID: mdl-38612814

ABSTRACT

Ag nanoparticles (AgNPs) were biosynthesized using sage (Salvia officinalis L.) extract. The obtained nanoparticles were supported on SBA-15 mesoporous silica (S), before and after immobilization of 10% TiO2 (Degussa-P25, STp; commercial rutile, STr; and silica synthesized from Ti butoxide, STb). The formation of AgNPs was confirmed by X-ray diffraction. The plasmon resonance effect, evidenced by UV-Vis spectra, was preserved after immobilization only for the sample supported on STb. The immobilization and dispersion properties of AgNPs on supports were evidenced by TEM microscopy, energy-dispersive X-rays, dynamic light scattering, photoluminescence and FT-IR spectroscopy. The antioxidant activity of the supported samples significantly exceeded that of the sage extract or AgNPs. Antimicrobial tests were carried out, in conditions of darkness and white light, on Staphylococcus aureus, Pseudomonas aeruginosa, Escherichia coli and Candida albicans. Higher antimicrobial activity was evident for SAg and STbAg samples. White light increased antibacterial activity in the case of Escherichia coli (E. coli) and Pseudomonas aeruginosa (P. aeruginosa). In the first case, antibacterial activity increased for both supported and unsupported AgNPs, while in the second one, the activity increased only for SAg and STbAg samples. The proposed antibacterial mechanism shows the effect of AgNPs and Ag+ ions on bacteria in dark and light conditions.


Subject(s)
Blood Group Antigens , Metal Nanoparticles , Antioxidants/pharmacology , Escherichia coli , Spectroscopy, Fourier Transform Infrared , Silver/pharmacology , Antigens, Fungal , Anti-Bacterial Agents/pharmacology , O Antigens , Silicon Dioxide , Plant Extracts/pharmacology
4.
Molecules ; 29(12)2024 Jun 09.
Article in English | MEDLINE | ID: mdl-38930815

ABSTRACT

Efficient separation of CH4 from N2 is essential for the purification of methane from nitrogen. In order to address this problem, composite materials consisting of rod-shaped SBA-15-based UiO-66-Br2 were synthesized for the purpose of separating a CH4/N2 mixture. The materials were characterized via PXRD, N2 adsorption-desorption, SEM, TEM, FT-IR, and TGA. The adsorption isotherms of CH4 and N2 under standard pressure conditions for the composites were determined and subsequently compared. The study revealed that the composites were formed through the growth of MOF nanocrystals on the surfaces of the SBA-15 matrix. The enhancements in surface area and adsorption capacity of hybrid materials were attributed to the structural modifications resulting from the interactions between surface silanol groups and metal centers. The selectivity of the composites towards a gas mixture of CH4 and N2 was assessed utilizing the Langmuir adsorption equation. The results of the analysis revealed that the U6B2S5/SBA-15 sample exhibited the greatest selectivity for CH4/N2 adsorption compared to the other samples, with an adsorption selectivity parameter (S) of 20.06. Additional research is necessary to enhance the enrichment of methane from CH4/N2 mixtures using SBA-15-based metal-organic framework materials.

5.
Mol Pharm ; 20(6): 2966-2977, 2023 06 05.
Article in English | MEDLINE | ID: mdl-37216314

ABSTRACT

Coenzyme Q10 is a potent antioxidant that plays an important role in the maintenance of various biochemical pathways of the body and has a wide range of therapeutic applications. However, it has low aqueous solubility and oral bioavailability. Mesoporous silica nanoparticles (MCM-41 and SBA-15 types) exhibiting varying pore sizes and modified with phosphonate and amino groups were used to study the influence of pore structure and surface chemistry on the solubility, in vitro release profile, and intracellular ROS inhibition activity of coenzyme Q10. The particles were thoroughly characterized to confirm the morphology, size, pore profile, functionalization, and drug loading. Surface modification with phosphonate functional groups was found to have the strongest impact on the solubility enhancement of coenzyme Q10 when compared to that of pristine and amino-modified particles. Phosphonate-modified MCM-41 nanoparticles (i.e., MCM-41-PO3) induced significantly higher coenzyme Q10 solubility than the other particles studied. Furthermore, MCM-41-PO3 led to a twofold decrease in ROS generation in human chondrocyte cells (C28/I2), compared to the free drug in a DMSO/DMEM mixture. The results confirmed the significant contribution of small pore size and negative surface charge of MSNs that enable coenzyme Q10 confinement to allow enhanced drug solubility and antioxidant activity.


Subject(s)
Antioxidants , Nanoparticles , Humans , Solubility , Antioxidants/pharmacology , Reactive Oxygen Species , Nanoparticles/chemistry , Silicon Dioxide/chemistry , Porosity , Drug Carriers/chemistry
6.
Nanotechnology ; 34(41)2023 Jul 24.
Article in English | MEDLINE | ID: mdl-37343532

ABSTRACT

In the current work, we report on the synthesizing of a series of novel nanocomposite materials obtained by functionalizing the SBA-15 silica matrix with anchored iron phosphonate molecules and the following thermal treatment. The obtained results reveal the formation of a unique amorphic layer of Fe-based compounds on the surface of silica walls of SBA-15 channels as a result of the organic groups' decomposition after moderate thermal treatment. Due to their unique structure, represented in an active Fe-containing amorphous coating spread over a large surface area, these materials are of great interest for their potential applications in fields such as catalysis, adsorption, and non-linear optics. The obtained materials remain amorphous, preserving the SBA-15 mesoporous structure up to temperatures of approximately 800 °C, after which the partial melting of the silica backbone is observed with the simultaneous formation of nanocrystals inside the newly-formed glassy mass. All obtained materials were characterized using such techniques as thermogravimetry, transmission and scanning electron microscopy combined with energy dispersive x-ray spectroscopy mapping, Raman spectroscopy, N2sorption analysis, x-ray diffraction, x-ray photoelectron spectroscopy, Mössbauer spectroscopy, and SQUID measurements.

7.
Environ Res ; 224: 115496, 2023 05 01.
Article in English | MEDLINE | ID: mdl-36796602

ABSTRACT

In this study, versatile boron-doped graphitic carbon nitride (gCN) incorporated mesoporous SBA-15 (BGS) composite materials were prepared by thermal polycondensation method using boric acid & melamine as a B-gCN source material and SBA-15 as mesoporous support. The prepared BGS composites are utilized sustainably using solar light as the energy source for the continuous flow of photodegradation of tetracycline (TC) antibiotics. This work highlights that the photocatalysts preparation was carried out with an eco-friendly strategy, solvent-free and without additional reagents. To alter the amount of boron quantity (0.124 g, 0.248 g, and 0.49 g) have to prepare three different composites using a similar procedure, the obtained composites viz., BGS-1, BGS-2 and BGS-3, respectively. The physicochemical property of the prepared composites was investigated by X-ray diffractometry, Fourier-transform infrared spectroscopy, Raman, Diffraction reflectance spectra, Photoluminescence, Brunauer-Emmett-Teller and transmission electron microscopy (TEM). The results shows that 0.24 g boron- loaded BGS composites degrade TC up to 93.74%, which is much higher than the rest of the catalyst. The addition of mesoporous SBA-15 incresed the specific surface area of the g-CN, and heteroatom of boron increased the interplanar stracking distance of g-CN, enlarged the optical absorption range, reducing the energy bandgap and enhanced the photocatalytic activity of TC. Additionally, the stability and recycling efficiency of the representative photocatalysts viz., BGS-2 was observed to be good even at the fifth cycle. The photocatalytic process using the BGS composites demonstrated to be capable candidate for the removal of tetracycline biowaste from aquesous media.


Subject(s)
Light , Nanocomposites , Boron , Tetracycline , Anti-Bacterial Agents , Nanocomposites/chemistry
8.
Int J Mol Sci ; 24(23)2023 Nov 29.
Article in English | MEDLINE | ID: mdl-38069280

ABSTRACT

A source of Brønsted acid centers, generated on the surface of two mesoporous silica supports of different structures (SBA-15 and MCF), was 3-(trihydroxysilyl)-1-propanesufonic acid (TPS). The materials obtained were characterized and applied as catalysts for the oxidative desulfurization of dibenzothiophene (DBT) with hydrogen peroxide as a model ODS (oxidative desulfurization) process. The properties of the materials were examined via nitrogen physisorption, XRD (X-ray Diffraction) and elemental analysis showing the preservation of the support structure after modification with organosilane species. Due to the aggregation of catalyst particles in the reaction mixture, the SBA-15 based catalyst was not very effective in DBT oxidation. Contrary, TPS/MCF catalyst exhibited a very good activity (almost total conversion of DBT after 1 h in optimized reaction conditions) and stability in dibenzothiophene oxidation in mild reaction conditions.


Subject(s)
Silicon Dioxide , Thiophenes , Oxidation-Reduction , Thiophenes/chemistry
9.
Int J Mol Sci ; 24(7)2023 Apr 04.
Article in English | MEDLINE | ID: mdl-37047711

ABSTRACT

The molecular dynamics of 1-butyl-3-methyl imidazolium tricyanomethanide ionic liquid [BMIM]+[TCM]- confined in SBA-15 mesoporous silica were examined using 1H NMR spin-lattice (T1) relaxation and diffusion measurements. An extensive temperature range (100 K-400 K) was considered in order to study both the liquid and glassy states. The hydrogen dynamics in the two states and the self-diffusion coefficients of the cation [BMIM]+ above the glass transition temperature were extracted from the experimental data. The results were then compared to the corresponding bulk substance. The effects of confinement on the dynamic properties of the ionic liquid clearly manifest themselves in both temperature regimes. In the high-temperature liquid state, the mobility of the confined cations reduces significantly compared to the bulk; interestingly, confinement drives the ionic liquid to the glassy state at a higher temperature Tg than the bulk ionic liquid, whereas an unusual T1 temperature dependence is observed in the high-temperature regime, assigned to the interaction of the ionic liquid with the silica-OH species.


Subject(s)
Ionic Liquids , Ionic Liquids/chemistry , Magnetic Resonance Spectroscopy , Magnetic Resonance Imaging , Silicon Dioxide , Cations
10.
Int J Mol Sci ; 24(3)2023 Jan 23.
Article in English | MEDLINE | ID: mdl-36768577

ABSTRACT

The aim of this study was to get insight into the pathway of the acetaldehyde formation from ethanol (the rate-limiting step in the production of 1,3-butadiene) on Cu-SBA-15 and Cu-MnSBA-15 mesoporous molecular sieves. Physicochemical properties of the catalysts were investigated by XRD, N2 ads/des, Uv-vis, XPS, EPR, pyridine adsorption combined with FTIR, 2-propanol decomposition and 2,5-hexanedione cyclization and dehydration test reactions. Ethanol dehydrogenation to acetaldehyde (without and with oxygen) was studied in a flow system using the FTIR technique. In particular, the effect of Lewis acid and basic (Lewis and BrØnsted) sites, and the oxygen presence in the gas reaction mixture with ethanol on the activity and selectivity of copper catalysts, was assessed and discussed. Two different reaction pathways have been proposed depending on the reaction temperature and the presence or absence of oxygen in the flow of the reagents (via ethoxy intermediate way at 593 K, in ethanol flow, or ethoxide intermediate way at 473 K in the presence of ethanol and oxygen in the reaction mixture).


Subject(s)
Copper , Ethanol , Ethanol/chemistry , Copper/chemistry , Oxygen , Acetaldehyde
11.
Molecules ; 28(6)2023 Mar 11.
Article in English | MEDLINE | ID: mdl-36985532

ABSTRACT

This paper reports the synthesis and structural analysis of mesoporous silica materials with the use of aluminum phyllosilicate clay (bentonite) as an alternative silica source. In the proposed synthesis, bentonite, as natural aluminosilicate, was used instead of commercially available and quite expensive tetraethyl orthosilicate (TEOS) silica source. The objective of the research study was to determine the effect of aluminum loading in the mesoporous silica body for ordering structure, porosity, and potential sorption capacity to thorium ions. The unique direction developed in this procedure is focused on preparing advanced materials from natural sources with their own desired functionality and general availability. The applied procedure based on the classic, one-step synthesis of SBA-15 silicates was modified by gradually increasing the bentonite amount with simultaneous reduction of the TEOS content. The structural and morphological characterization, as well as evaluation of the porous structure of the obtained materials, was performed using powder wide-angle X-ray diffraction (XRD), small-angle scattering (SAXS), transmission and scanning electron microscopy (TEM, SEM), low-temperature nitrogen adsorption-desorption methods and potentiometric titration. The new, cost-effective composites for the removal of Th(IV) ions are proposed. The synergistic effect of expanding the porous surface using bentonite as a silica precursor and the presence of thorium-binding groups (such as Al2O3) is indicated.

12.
Molecules ; 28(11)2023 May 23.
Article in English | MEDLINE | ID: mdl-37298738

ABSTRACT

In this study, nanocomposites based on polypropylene are synthesized by the in situ polymerization of propene in the presence of mesoporous SBA-15 silica, which acts as a carrier of the catalytic system (zirconocene as catalyst and methylaluminoxane as cocatalyst). The protocol for the immobilization and attainment of hybrid SBA-15 particles involves a pre-stage of contact between the catalyst with cocatalyst before their final functionalization. Two zirconocene catalysts are tested in order to attain materials with different microstructural characteristics, molar masses and regioregularities of chains. Some polypropylene chains are able to be accommodated within the silica mesostructure of these composites. Thus, an endothermic event of small intensity appears during heating calorimetric experiments at approximately 105 °C. The existence of these polypropylene crystals, confined within the nanometric channels of silica, is corroborated by SAXS measurements obtained via the change in the intensity and position of the first-order diffraction of SBA-15. The incorporation of silica also has a very significant effect on the rheological response of the resultant materials, leading to important variations in various magnitudes, such as the shear storage modulus, viscosity and δ angle, when a comparison is established with the corresponding neat iPP matrices. Rheological percolation is reached, thus demonstrating the role of SBA-15 particles as filler, in addition to the supporting role that they exert during the polymerizations.


Subject(s)
Nanocomposites , Polypropylenes , Polymerization , Polypropylenes/chemistry , Metallocenes , Molecular Weight , Scattering, Small Angle , X-Ray Diffraction , Nanocomposites/chemistry , Silicon Dioxide/chemistry
13.
Molecules ; 29(1)2023 Dec 22.
Article in English | MEDLINE | ID: mdl-38202685

ABSTRACT

Optimized sustainable procedures in both acidic and basic conditions are considered to meet some of the current environmental challenges of the scientific community. In this paper, the successful syntheses of two classes of indium-based silica nanomaterials are reported. Both procedures were conceived to enhance the sustainability of the synthesis methods and promote their preparations at room temperature while avoiding the hydrothermal treatment under static conditions at 100 °C. A fast, room-temperature synthesis of porous nanospheres was conceived together with an "acid-free" procedure for SBA-15-like materials. Moreover, the isomorphic substitution of silicon with indium was achieved. All the materials were deeply characterized to probe their structural, textural and morphological properties (e.g., transmission electron microscopy, N2 physisorption, ss MAS NMR of 29Si). The high specific surface area and the mesoporosity were always preserved even under the mild reaction conditions employed. The honeycomb structure and the spherical morphology of SBA-15-like materials and nanospheres, respectively, were also observed. The insertion of indium was confirmed via X-ray photoelectron spectroscopy (XPS) investigations.

14.
Molecules ; 28(6)2023 Mar 08.
Article in English | MEDLINE | ID: mdl-36985454

ABSTRACT

A survey was designed to investigate the pesticide residues in agricultural produce and to estimate their potential intake risks to inhabitants. A total of 314 samples of nine types of fruits and vegetables were collected from the supermarkets and vegetable markets of Shandong Province (China) from October 2020 to February 2022. An accurate and reliable multi-residue method, based on GC-MS/MS detection, as well as the multiplug filtration cleanup method, based on SBA-15-C18, was prepared by a solution chemical reaction. Additionally, an in situ co-condensation method was established for the quantification of 139 pesticide residues. Residues that contained no pesticides were detected in 66.5% of the 314 samples. Moreover, of the samples, 30.6% were at or below the MRLs, and 2.9% were above the MRLs. Residues of procymidone were found to be the one that most often exceeded the MRLs (1.3% of the samples). Tebuconazole was found most frequently in 22.0% of the samples analyzed. Consumer exposure to the 139 pesticides did not exceed 100% ADI and ARfD. This led to a consideration that these pesticide residues in the nine commodities may not raise the health risk of the consumers in the long and short term. The highest value of chronic dietary intake was obtained from spirodiclofen, which resulted in a 24.1% of ADI. Furthermore, the highest exposure levels in the short term were obtained from the consumption of leeks with procymidone (58.3% ARfD).


Subject(s)
Pesticide Residues , Pesticides , Pesticides/analysis , Pesticide Residues/analysis , Tandem Mass Spectrometry , Gas Chromatography-Mass Spectrometry , Food Contamination/analysis , Vegetables/chemistry , Risk Assessment , Eating
15.
Chemistry ; 28(66): e202202105, 2022 Nov 25.
Article in English | MEDLINE | ID: mdl-35998025

ABSTRACT

Herein, the synthesis of a new type of catalyst, SBA-M (Schiff complex of different metal types grafted on SBA-15) based on a quaternization reaction, is described. Various amounts of ionic liquid were grafted into the pore channels of SBA-15 using the post-grafting method, which allowed the ionic liquid to be grafted into the pore channels restrictively. Notably, over six cycles, SBA-Mn (0.2) has been shown to maintain its catalytic activity and stability. In addition, a reaction mechanism for the cycloaddition of CO2 with epoxides based on density-functional theory is proposed. The cycloaddition reaction of CO2 and epoxides is an efficient way of carbon fixation. It is demonstrated that the metal coordinated with the oxygen atom of the epoxides and that a halogen attacked the carbon of epoxides. Moreover, theoretical calculations and synthesis strategy provide a new approach for CO2 conversion.

16.
Mol Pharm ; 19(4): 1091-1103, 2022 04 04.
Article in English | MEDLINE | ID: mdl-35238208

ABSTRACT

SBA-15 mesoporous silica (MPS) has been widely used in oral drug delivery; however, it has not been utilized for solidifying lipid-based formulations, and the impact of their characteristic intrawall microporosity remains largely unexplored. Here, we derive the impact of the MPS microporosity on the in vitro solubilization and in vivo oral pharmacokinetics of the prostate cancer drug abiraterone acetate (AbA) when coencapsulated along with medium chain lipids into the pores. AbA in lipid (at 80% equilibrium solubility) was imbibed within a range of MPS particles (with comparable morphology and mesoporous structure but contrasting microporosity ranging from 0-247 m2/g), and their solid-state properties were characterized. Drug solubilization studies during in vitro lipolysis revealed that microporosity was the key factor in facilitating AbA solubilization by increasing the surface area available for drug-lipid diffusion. Interestingly, microporosity hindered hydrolysis of AbA to its active metabolite, abiraterone (Ab), under simulated intestinal conditions. This unique relationship between microporosity and AbA/Ab aqueous solubilization behavior was hypothesized to have significant implications on the subsequent bioavailability of the active metabolite. In vivo oral pharmacokinetics studies in male Sprague-Dawley rats revealed that MPS with moderate microporosity attained the highest relative bioavailability, while poor in vitro-in vivo correlations (IVIVC) existed between in vitro drug solubilization during lipolysis and in vivo AUC. Despite this, a reasonable IVIVC was established between the in vitro solubilization and in vivoCmax, providing evidence for an association between silica microporosity and oral drug absorption.


Subject(s)
Abiraterone Acetate , Lipids , Abiraterone Acetate/chemistry , Administration, Oral , Animals , Biological Availability , Lipids/chemistry , Male , Rats , Rats, Sprague-Dawley , Silicon Dioxide/chemistry , Solubility
17.
Environ Sci Technol ; 56(6): 3678-3688, 2022 03 15.
Article in English | MEDLINE | ID: mdl-35195408

ABSTRACT

Catalytic ozonation of methyl mercaptan (CH3SH) can effectively control this unbearable odorous sulfur-containing volatile organic compound (S-VOC). The construction of an electronic metal-support interaction (EMSI) coordination structure to maximize the number of active sites and increase the intrinsic activity of active sites is an effective means to improve catalytic performance. In this work, the abundant Si-OH groups on PSBA-15 (SBA-15 before calcination) were used to anchor Mn to form a Si-O-Mn-based EMSI coordination structure. Detailed characterizations and theoretical simulations reveal that the strong EMSI effect significantly adjusts and stabilizes the electronic structure of Mn 3d states, resulting in an electron-rich center on the Si-O-Mn bond to promote the specific adsorption/activation of ozone (O3) and an electron-poor center on the (Si-O-)Mn-O bond to adsorb a large amount of CH3SH accompanied by its own oxidative degradation. In situ Raman and in situ Fourier transform infrared (FTIR) analyses identify that catalytic ozonation over 3.0Mn-PSBA generates atomic oxygen species (AOS/*O) and reactive oxygen species (ROS/•O2-) to achieve efficient decomposition of CH3SH into CO2/SO42-. Furthermore, the electrons obtained from CH3SH in electron-poor centers are transferred to maintain the redox cycle of Mn2+/3+ → Mn4+ → Mn2+/3+ through the internal bond bridge, thus accomplishing the efficient and stable degradation of CH3SH prolonged to 180 min. Therefore, the rational design of catalysts with abundant active sites and optimized inherent activity via the EMSI effect can provide significant potential to improve catalytic performance and eliminate odorous gases.

18.
Environ Res ; 204(Pt D): 112383, 2022 03.
Article in English | MEDLINE | ID: mdl-34813864

ABSTRACT

Cobalt oxide (Co3O4) is a low-cost material exhibiting excellent physicochemical and photocatalytic properties indicating its potential use for next-generation eco-friendly energy storage and photocatalytic degradation applications. In this study, Co3O4 nanoarcs were synthesized using SBA-15 as a template by microwave-assisted method to form an S15/m-Co3O4 product. Characterization was done by low and wide-angle X-Ray diffraction, and Fourier transformed infra-red spectroscopic studies confirming the presence of S15/m-Co3O4. Scanning Electron Microscope images proved the agglomerated nanotube and nanoarcs like the structure of SBA-15 and S15/m- Co3O4, respectively. Electrochemical studies included cyclic voltammetry, charge/discharge, retention capacity, and electron impedance spectroscopy studies in a 3-electrode system. S15/m-Co3O4 nanoarcs, as the electrode material, was revealed to have a specific capacity of 87.5 C/g in 1 M KOH solution. Upon running 1000 cycles, the material had excellent capacity retention of 87%. The S15/m-Co3O4 product also underwent photocatalytic degradation studies. The Rhodamine R6G dye degradation by S15/m-Co3O4 under UV irradiation exhibited a high degradation percentage of 97.7%, following the first-order kinetics. S15/m-Co3O4 has proven to be biocompatible and can be used to enhance supercapacitors which are an ideal alternative to conventional batteries for energy storage applications. Thus, the data produced proves S15/m-Co3O4 nanoarcs is an excellent electrode material for pseudocapacitive application and a catalyst for photocatalytic degradation of dye molecules.


Subject(s)
Oxides , Catalysis , Cobalt , Electrodes , Oxides/chemistry , Silicon Dioxide
19.
Biologicals ; 80: 18-26, 2022 Oct.
Article in English | MEDLINE | ID: mdl-36414490

ABSTRACT

Routine immunization against diphtheria and tetanus has drastically reduced the incidence of these diseases worldwide. Anti-diphtheria/tetanus vaccine has in general aluminum salt as adjuvant in its formulation that can produce several adverse effects. There is a growing interest in developing new adjuvants. In this study, we evaluated the efficiency of SBA-15 as an adjuvant in subcutaneous immunization in mice with diphtheria (dANA) and tetanus (tANA) anatoxins as well as with the mixture of them (dtANA). The tANA molecules and their encapsulation in SBA-15 were characterized using Small-Angle X-ray Scattering (SAXS), Dynamical Light Scattering (DLS), Nitrogen Adsorption Isotherm (NAI), Conventional Circular Dichroism (CD)/Synchrotron Radiation Circular Dichroism (SRCD) Spectroscopy, and Tryptophan Fluorescence Spectroscopy (FS). The primary and secondary antibody response elicited by subcutaneous immunization of High (HIII) and Low (LIII) antibody responder mice with dANA, tANA, or dtANA encapsulated in the SBA-15 were determined. We demonstrated that SBA-15 increases the immunogenicity of dANA and tANA antigens, especially when administered in combination. We also verified that SBA-15 modulates the antibody response of LIII mice, turning them into high antibody responder. Thus, these results suggest that SBA-15 may be an effective adjuvant for different vaccine formulations.


Subject(s)
Diphtheria , Tetanus , Mice , Animals , Immunity, Humoral , Scattering, Small Angle , X-Ray Diffraction , Diphtheria/prevention & control , Tetanus/prevention & control , Tetanus Toxoid , Silicon Dioxide/pharmacology , Adjuvants, Immunologic/pharmacology , Immunization, Secondary/methods , Antibodies, Bacterial
20.
Bioprocess Biosyst Eng ; 45(6): 1075-1088, 2022 Jun.
Article in English | MEDLINE | ID: mdl-35532819

ABSTRACT

A series of nickel-incorporated SBA-15 mesoporous molecular sieves (Ni-SBA-15) were prepared as support for the immobilization of his-tagged recombinant Microbacterium esterase. The Ni-SBA-15 could strongly and specific absorb the his-tagged esterase from cell disrupted supernatant. It was found that the nickel amount in Ni-SBA-15 has dramatic influence on the activity and thermo-stability of immobilized enzyme, while the kinds of nickel precursor had little effect on enzyme stability. The morphology, chemical composition and structure of the best support NiCl2-SBA-15 (Ni-SBA-15 prepared from NiCl2 precursor) were characterized by various spectroscopy techniques. The immobilized esterase retained full activity of free esterase and showed high immobilized yield (> 90%) with higher thermo-stability, pH stability and organic solvent resistance compared with free enzyme. The optimum reaction temperature increased from 35 to 40 °C and the optimal reaction pH moved from 10.0 to 8.0 after enzyme immobilization. The immobilized esterase exhibited excellent storage stability and keeping 92% of the initial activity after 30 days' storage at 25 °C. In addition, the immobilized esterase had excellent reusability for the synthesis of key chiral intermediate of d-biotin and the substrate conversion could still keep 100% after 13 cycles continuously. Finally, optical pure (4S, 5R)-hemiester was obtained in 80.8% isolated yield and 99% purity in the gram preparative scale.


Subject(s)
Biotin , Esterases , Biotin/metabolism , Enzyme Stability , Enzymes, Immobilized/chemistry , Hydrogen-Ion Concentration , Microbacterium , Nickel/chemistry , Silicon Dioxide/chemistry , Temperature
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