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1.
J Environ Manage ; 330: 117206, 2023 Mar 15.
Artigo em Inglês | MEDLINE | ID: mdl-36621312

RESUMO

The increasing usage of phosphate fertilizers for agricultural purposes has led to an augmented level of phosphorus in watercourses negatively impacting the ecosystems and water quality warranting its amputation from polluted water. This article describes the preparation of a novel natural deep eutectic solvent (NADES) functionalized-celite/polyethylene glycol hydrogel nanocomposite (NADES-Cel/PEG HNC) for adsorptive phosphate removal from water. The XRD, FTIR, SEM coupled with EDX spectroscopy, TEM, BET analysis, and pHpzc measurement were used to characterise the prepared material. Central composite design (CCD) in response surface methodology (RSM) was used for experimental design to analyse the individual and combined impact of five operational parameters on equilibrium adsorption capacity (Qe), and evaluate the optimal operating conditions by numerical optimization, which were obtained as: contact time (60 min), adsorbent dosage (1.0 g/L), initial [PO43-] (80 mg/L), initial solution pH (3.5), and temperature (304 K). The adsorption process was best explicated via Langmuir adsorption isotherm with a noteworthy saturation capacity, Qm of 111.80 mg PO43-/g at 298 K, and was favourable (S* = 0.99), feasible (ΔG° = -7.02 kJ/mol), exothermic (ΔH° = -8.39 kJ/mol) and physical in nature. The uptake mechanism largely involved H-bonding, electrostatic interaction, n-π interaction and pore-filling. Uptake kinetics of PO43- was best explicated by pseudo-second order model, and the rate-determining step involved both intraparticle and liquid film diffusion mechanisms. The admirable performance of NADES-Cel/PEG HNC was signified by its competent adsorption efficacy and effectual reusability. The pertinence of the hydrogel nanocomposite for treatment of real wastewater was tested. Hence, NADES-Cel/PEG HNC might prove to be a pragmatic adsorbent for decontamination of PO43- from an aqueous environment.


Assuntos
Nanocompostos , Poluentes Químicos da Água , Termodinâmica , Terra de Diatomáceas , Solventes Eutéticos Profundos , Solventes , Adsorção , Fosfatos , Projetos de Pesquisa , Ecossistema , Materiais Biocompatíveis , Cinética , Nanocompostos/química , Glicina , Polietilenoglicóis , Frutose , Poluentes Químicos da Água/química , Concentração de Íons de Hidrogênio
2.
Environ Res ; 220: 115193, 2023 03 01.
Artigo em Inglês | MEDLINE | ID: mdl-36587717

RESUMO

The purpose of the study was to fabricate sustainable and cost-effective material for the thorough cleansing of polluted water. In this context, an economical, phytogenic and multifunctional Origanum vulgare plant-based nanocomposite material, MnFe2O4/OV, was prepared via one-pot synthetic technique. The synthesized nanocomposite with a band gap of 2.02 eV behaved as an efficient nano-photocatalyst for the degradation of both cationic (crystal violet) and anionic (congo red) dyes under direct sunlight irradiation. The material also inhibited the growth of E. coli and S. aureus bacteria and simultaneously adsorbed both cationic and anionic dyes from water through adsorption. A variety of techniques have been used to characterize the nanocomposite, including X-ray powder diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX) and transmission electron microscopy (TEM). Additionally, the kinetics of photodegradation of the aforementioned organic dyes has also been investigated. The MnFe2O4/OV exhibited excellent photocatalytic performance, leading to 43% and 72% degradation within 3 h at rate constants of 2.0 × 10-3 min-1 and 6.0 × 10-3 min-1 for crystal violet and congo red, respectively. The crystal violet and congo red were used to testify to the composite's potential for adsorption under the influence of several process variables, including initial solution pH, contact time, temperature, initial dye concentration, and amount of MnFe2O4/OV. The Langmuir maximum adsorption capacity Qmax as in the range 14.06-14.59 mgg-1 for crystal violet and 34.45-23.93 mgg-1 for congo red at pH 7 within 90 min contact time in the temperature range of 30-50 °C. The phenomenon of adsorption was found feasible and endothermic at all the investigated temperatures. Also, E. coli and S. Aureus bacteria have shown growth suppression activity when exposed to MnFe2O4/OV.As a result, the synthesized nanocomposite, MnFe2O4/OV, proved to be an antimicrobial, multifunctional novel nanocomposite, which is in high demand, and could serve as an affordable, and sustainable material for comprehensive water filtration.


Assuntos
Nanocompostos , Origanum , Corantes/química , Vermelho Congo/farmacologia , Staphylococcus aureus , Escherichia coli , Violeta Genciana/farmacologia , Água/química , Nanocompostos/química , Adsorção
3.
Sci Rep ; 12(1): 14656, 2022 08 29.
Artigo em Inglês | MEDLINE | ID: mdl-36038589

RESUMO

In recent times, biopolymer-metal oxide nanocomposites have gained prominent importance in the attenuation of environmental toxicants from aqueous phase. But lanthanide oxide-based biopolymer nanocomposites have scantly been evaluated for their adsorption potential. A novel guar gum-polyacrylamide/erbium oxide nanocomposite (GG-PAAm/Er2O3 NC) adsorbent was synthesized by copolymerization of guar gum (GG) and acrylamide (AAm) utilizing N-N'-methylenebisacrylamide as a crosslinker and Er2O3 as a reinforcing agent. The adsorptive efficacy of GG-PAAm/Er2O3 nanocomposite was evaluated using nile blue (NB) as a model pollutant dye from aquatic system. The prepared adsorbent was characterized by Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD) analysis, Brunauer-Emmett-Teller (BET) analysis, thermogravimetric analysis, scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDX), and high-resolution transmission electron microscopy (HRTEM). The optimal process parameters, which include dosage (0.8 g/L), agitation time (40 min), initial solution pH (6), and initial NB concentration (80 mg/L) were determined by batch methodology. The equilibrium data for NB confiscation was better expressed by Langmuir isotherm model, with maximal adsorption effectiveness (Qm) of 225.88 mg NB/g demonstrating the actively monolayer adsorption onto homogeneous surface of GG-PAAm/Er2O3 NC. The kinetics of NB sorption process onto GG-PAAm/Er2O3 NC was reliable with pseudo-second order model. Thermodynamic parameters such as ΔH° (15-17 kJ/mol) and ΔS° (0.079-0.087 kJ/mol/K), and - ΔG° (8.81-10.55 kJ/mol) for NB validated the endothermic, an increased randomness at the GG-PAAm/Er2O3-NB interface, and spontaneity and feasibility of the process, respectively. The spent nanocomposite was effectively regenerated with NaOH, and could be reused proficiently for five runs demonstrating the high reusability potential of the nanocomposite. The commendable removal efficiency and high reusability of GG-PAAm/Er2O3 NC recommended it to be a highly competent adsorbent for cationic dyes particularly NB diminution from aqueous waste.


Assuntos
Nanocompostos , Poluentes Químicos da Água , Resinas Acrílicas , Adsorção , Corantes/análise , Érbio , Galactanos , Concentração de Íons de Hidrogênio , Cinética , Mananas , Nanocompostos/química , Oxazinas , Óxidos , Gomas Vegetais , Espectroscopia de Infravermelho com Transformada de Fourier , Termodinâmica , Água , Poluentes Químicos da Água/análise
4.
Langmuir ; 38(27): 8280-8295, 2022 07 12.
Artigo em Inglês | MEDLINE | ID: mdl-35758902

RESUMO

In the present investigation, a novel, green, and economical dual-functionalized pullulan/kaolin hydrogel nanocomposite (f-PKHN) was fabricated and subsequently applied for the liquid-phase decontamination of paracetamol (PCT), a pharmaceutical pollutant. Pullulan and kaolin were functionalized with l-asparagine and gallic acid, respectively. The physicochemical facets of the functionalized pullulan/kaolin hydrogel nanocomposite and its interactive behavior with PCT were elucidated by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDX), and elemental mapping. The process parameters along with the isotherm, kinetics, and thermodynamics were methodically appraised via a batch technique to unveil the adsorption performance of the as-fabricated hydrogel nanocomposite. The adsorption isotherm and kinetics of PCT uptake by f-PKHN conform well to Freundlich and pseudo-second-order models, respectively. Relying on hydrogen bonding, n-π, and van der Waals interactions, the maximum adsorption capacity was 332.54 mg g-1, higher than for most of the previous adsorbents reported in the literature for PCT removal. Thermodynamic calculations corroborated endothermic, spontaneous, and feasible adsorption phenomena. The maintenance of a high uptake percentage (69.11%) in the fifth consecutive adsorption-desorption cycle implied the significant reusable potential of f-PKHN. Swelling studies exhibited 90% swelling within 200 min, indicating the successful fabrication of a cross-linked hydrogel network. The real water (distilled water, tap water, and river water) samples spiked with PCT specified a significant uptake of PCT (>85%), and the minor influence of ionic strength on the adsorptive potential of f-PKHN validated its potentiality for the decontamination of real effluents. In conclusion, f-PKHN with substantial adsorption capacity, green characteristics, and excellent reusability can be reckoned with as a promising adsorbent for the de-escalation of PCT from aquatic sources as well as at the industrial level.


Assuntos
Nanocompostos , Poluentes Químicos da Água , Acetaminofen , Adsorção , Glucanos , Hidrogéis , Concentração de Íons de Hidrogênio , Caulim , Cinética , Nanocompostos/química , Espectroscopia de Infravermelho com Transformada de Fourier , Termodinâmica , Águas Residuárias/química , Água , Poluentes Químicos da Água/análise
5.
Environ Res ; 213: 113712, 2022 10.
Artigo em Inglês | MEDLINE | ID: mdl-35718168

RESUMO

The adsorption of acridine orange and Cr6+ ion onto plaster of paris reinforced glutamic acid-grafted-polyacrylamide hydrogel nanocomposite modified with riboflavin, Glu-g-PAM/POP/Rb HNC was studied. The Glu-g-PAM/POP/Rb HNC was physico-chemically characterized by Fourier transform infrared spectroscopy, X-ray diffraction analysis, scanning electron microscopy coupled with energy dispersive X-ray spectroscopy, transmission electron microscopy and Brunauer-Emmett-Teller analysis. The specific surface area, pore volume and pore diameter were 15.48 m2/g, 0.015 cm3/g and 4.23 nm, respectively. Adsorption process was strategized by response surface methodology (RSM) based on a 3-level 5-factor (initial solution pH, contact time, adsorbent dose, initial adsorbate concentration and temperature) central composite design (CCD), and validity of the estimated parameters was statistically evaluated using analysis of variance (ANOVA). The optimized operating variables were: pH (AO = 10; Cr6+ = 4.15), contact time (AO = 60 min; Cr6+ = 59 min), adsorbent dose (0.8 g/L), initial adsorbate concentration (60 mg/L) and temperature (298 K). Isotherm results were coincident with Langmuir isotherm model. The experimental kinetic adsorption data was congruous with pseudo-second order model, with the uptake rate controlled by both intraparticle and liquid film diffusions. The relatively high Langmuir saturation capacity of 202.63 mg AO/g and 143.68 mg Cr6+/g, supported by the decent recyclability up to four times affirmed the promising performance of the adsorbent. The efficacy of the adsorbent for simultaneous removal of AO and Cr6+ from bi-component system was assessed. The possible adsorption mechanism mainly involved hydrogen bonding, van der Waals forces, electrostatic and π-π interactions. Adsorption of AO and Cr6+ onto Glu-g-PAM/POP/Rb HNC was feasible and exothermic as revealed by the thermodynamic parameters. The findings demonstrated superior adsorbent efficacy for the seizure of pollutants, particularly AO and Cr6+ from aqueous solution.


Assuntos
Nanocompostos , Poluentes Químicos da Água , Laranja de Acridina/análise , Laranja de Acridina/química , Resinas Acrílicas , Adsorção , Sulfato de Cálcio , Ácido Glutâmico , Hidrogéis , Concentração de Íons de Hidrogênio , Cinética , Riboflavina/análise , Espectroscopia de Infravermelho com Transformada de Fourier , Termodinâmica , Poluentes Químicos da Água/análise
6.
Bioresour Technol ; 354: 127168, 2022 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-35436542

RESUMO

Printing and dyeing wastewater (PDW) has characteristics of large amount of water, elevated content of residual dyes, poor biodegradability, high alkalinity and large change of water quality, making its treatment difficult. Development of efficient and economic PDW treatment technology has gained considerable interest in the field of environmental protection. Use of plant biomass carbon (PBC) for the adsorption of dyes is a feasible and economical technology. This review summarizes current literature discussing the preparation method and physicochemical characteristics of PBC prepared from different plant species, the effect of PBC on the removal of dyes, influencing factors affecting the removal, and relevant adsorption models. The shortcomings of current research and the direction of future research are also pointed out in the review.


Assuntos
Poluentes Químicos da Água , Purificação da Água , Adsorção , Biomassa , Carbono , Corantes/química , Águas Residuárias/química , Poluentes Químicos da Água/análise
7.
Int J Phytoremediation ; 24(11): 1173-1183, 2022.
Artigo em Inglês | MEDLINE | ID: mdl-34990566

RESUMO

Herein, a magnetic biochar adsorbent based on Pyrus pyrifolia discarded peels impregnated with precursor FeCl3·6H2O was fabricated and probed as a low-cost adsorbent for toxic cationic dye methylene blue (MB). The textural characterization of Pyrus pyrifolia magnetic biochar (PMBC) obtained from BET analysis exhibited its mesoporous nature with SBET of 133.960 m2/g. The physicochemical characteristics of PMBC were elucidated using XRD, FTIR, SEM-EDX and TEM techniques. The impregnation of FeCl3 has a significant impact on the microstructure of Pyrus pyrifolia based biochar which resulted in enhancement in adsorption efficiency of PMBC. The sorption parameters adsorbent dosage, time, initial MB concentration, and pH were thoroughly elucidated using a batch methodology which were found to be 0.8 g/L, 40 min, 90 mg/L and 6, respectively. Temkin and pseudo-second-order rate equation respectively appropriated the equilibrium data than the rest of the models. The maximum adsorption capacity determined by the Langmuir model was found to be 967.80 mg/g. The adsorbent exhibited better regeneration up to 3 cycles validating its practical usage. The facile synthesis, economic, and environmentally benign characteristic of Pyrus pyrifolia magnetic biochar corroborated it as a highly efficient adsorbent to sequester MB from an aqueous phase.


Pyrus pyrifolia discarded peels impregnated with FeCl3·6H2O were exploited as a novel magnetic biosorbent for the abatement of cationic dye from wastewater. The impact of operative variables was analyzed using batch methodology. Isotherm and kinetic modeling on equilibrium data was executed via non-linear approach which is very reliable in comparison to linear way.


Assuntos
Pyrus , Poluentes Químicos da Água , Adsorção , Biodegradação Ambiental , Carvão Vegetal , Concentração de Íons de Hidrogênio , Ferro , Cinética , Azul de Metileno/química , Água , Poluentes Químicos da Água/química
8.
Chemosphere ; 289: 133232, 2022 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-34896178

RESUMO

Herein, a functionalized green hydrogel nanocomposite based on carboxymethylated gum tragacanth and nanobentonite (GTBCH) was designed via free-radical polymerization approach for the elimination of Aspartame (AS) from wastewater. The GTBCH fabrication was validated by Fourier Transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Transmission electron microscopy (TEM), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDX) techniques. Central composite design (CCD) was efficaciously applied to determine the quadratic polynomial approach for predicting the adsorption capacity (qe) of AS. The optimum sequestration conditions were dosage (0.8 g L‒1), agitation time (35 min) initial AS concentration (60 mg L-1), pH (6) and temperature (308 K). The CCD results revealed that dosage of GTBCH and initial concentration have greater impact on qe followed by pH, time, and temperature. The significant adsorption capacity (392.04 mg g-1), calculated from Langmuir model, could be attributed to the stronger interactions prevalent between AS and GTBCH. Diffusion investigations depicted the uptake of AS via surface adsorption, liquid film and intraparticle diffusion, respectively. Ionic strength and real water have minor effect on the adsorption capacity demonstrating electrostatic interaction has least impact in adsorption process. The pHzpc, FTIR and XPS investigations revealed hydrogen bonding, n-π and van der Waals interactions as the principal removal mechanisms. Robust design, high adsorption capacity, eco-friendly facets along with excellent reusability indicated the GTBCH as a competent adsorbent for AS decontamination from wastewater.


Assuntos
Nanocompostos , Poluentes Químicos da Água , Adsorção , Aspartame , Hidrogéis , Concentração de Íons de Hidrogênio , Cinética , Espectroscopia de Infravermelho com Transformada de Fourier , Água
9.
J Org Chem ; 86(21): 15096-15116, 2021 Nov 05.
Artigo em Inglês | MEDLINE | ID: mdl-34586815

RESUMO

A highly controlled DDQ-catalyzed oxidative C(sp3)-H functionalization of three contiguous carbon atoms in aryltetralins is reported for efficient access to diverse oxygenated dihydronaphthalene scaffolds. The first total synthesis of pachypostaudin B is realized. Further, a CAN-mediated chemoselective oxidative demethylation on the dihydronaphthalene scaffolds is demonstrated to arrive at the rarely observed dihydronaphthoquinone core in moderate to good yields. The present methodology enables quick access to a library of magnoshinin and merrilliaquinone analogs.

10.
Environ Sci Pollut Res Int ; 28(38): 53298-53313, 2021 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-34031821

RESUMO

Herein, kaolin (K) was amended by a novel gemini surfactant to attain nano-kaolin (nK), which was subsequently employed as a cross-linker in the preparation of itaconic acid/kaolin hydrogel nanocomposite (IA/nK) via free radical polymerization route employing the sonochemical technique, which has been used for the first time to extract metformin (MF) from water solution. The aspects which affect sorption behavior of IA/nK on metformin (MF) were systematically investigated via batch experiments, in harmony with effect of sorbent dosage, contact time, pH, MF concentration, equilibrium curves, kinetic behavior, and thermodynamic parameters. BET studies of IA/nK exhibited SBET of 106.42 m2g-1, pore volume 0.281 cm3 g-1, and a pore radius of 16.627 Å. Kinetic and isotherm modelling portrayed that pseudo-second order and Freundlich model appropriated adsorption data with maximum sorption capacity of 278.35 mg g-1. Thermodynamic parameters ΔHO (13.67 kJmol-1) and ΔGO (-7.648 kJmol-1) revealed that sequestration of MF on IA/nK was endothermic, spontaneous, and dominated by physisorption. Molecular docking study along with X-ray photoelectron spectroscopy inferred electrostatic interaction and hydrogen bonding as main mechanism of MF removal. IA/nK demonstrated dose-reliant inhibition of both gram-positive and gram-negative bacterial strains. IA/nK demonstrated good regeneration properties, up to four cycles without considerable decrease in its efficacy. The admirable sorption capacity coupled with good reusability, and low toxicity substantiates IA/nK as promising adsorbent for MF confiscation.


Assuntos
Metformina , Nanocompostos , Poluentes Químicos da Água , Adsorção , Hidrogéis , Concentração de Íons de Hidrogênio , Caulim , Cinética , Simulação de Acoplamento Molecular , Succinatos , Termodinâmica
11.
ACS Omega ; 5(6): 2843-2855, 2020 Feb 18.
Artigo em Inglês | MEDLINE | ID: mdl-32095706

RESUMO

Herein, a simplistic redox polymerization strategy was utilized for the fabrication of a poly(methacrylic acid)/montmorillonite hydrogel nanocomposite (PMA/nMMT) and probed as a sorbent for sequestration of two pharmaceutical contaminants, viz., amoxicillin (AMX) and diclofenac (DF), from wastewater. The synthesized hydrogel nanocomposite was characterized by the Fourier transform infrared, X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy-energy dispersive X-ray spectroscopy, and transmission electron microscopy techniques to analyze structural characteristics and sorption interactions. The efficacy of PMA/nMMT was thoroughly investigated for the sequestration of AMX and DF from the aquatic phase with a variation in operative variables like agitation time, sorbent dosage, pH, and initial sorbate concentration. The reaction kinetics was essentially consistent with the pseudo-second-order model with rate dominated by the intraparticle diffusion model as well as the film diffusion mechanism. The Freundlich isotherm appropriated the equilibrium data over the entire range of concentration. Thermodynamic investigation explored the spontaneous and endothermic nature of the process. The most possible mechanism has been explained, which includes electrostatic interaction, hydrogen bonding, cationic exchange, and partition mechanism. Economic feasibility, better sorption capacity (152.65 for AMX and 152.86 mg/g for DF), and efficient regeneration and reusability even after four consecutive sorption-desorption cycles ascertained PMA/nMMT as a potential sorbent for AMX and DF uptake from the aqueous phase.

12.
Ultrason Sonochem ; 60: 104761, 2020 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-31499323

RESUMO

Clay-hydrogel nanocomposites are suitable material for mitigating the pollution/environmental impact because of their high adsorption capacity. In this study, the synthesis of polyacrylamide/bentonite hydrogel nanocomposite was assisted by ultrasound through successful incorporation of nanobentonite as filler and cross-linker into polyacrylamide framework. The adsorbent was characterized by FTIR, XRD, BET, SEM-EDX, and TEM in order to observe structural changes and sorption interactions. The effect of adsorbent dose, contact time, initial metal ion concentration and pH on the sequestration of Pb2+ and Cd2+ was analyzed. The adsorbent removed more than 95% Pb2+ and Cd2+ within first 20 min, which corresponds to relatively high pseudo-first order rate constant, k1 (0.240 for Pb2+ and 0.253 1/min for Cd2+) and pseudo-second order rate constant, k2 (0.031 for Pb2+ and 0.033 g/mg/min for Cd2+). The isotherm and kinetics modeling data were best described by Freundlich isotherm over the entire concentration range and pseudo-second order rate equation, respectively. The thermodynamic studies implied spontaneous and endothermic nature of adsorption process. The maximum adsorption capacity (138.33 for Pb2+ and 200.41 mg/g for Cd2+) determined using Langmuir model along with a good regeneration potential depicts that polyacrylamide/bentonite hydrogel nanocomposite could be used effectively for Pb2+ and Cd2+ uptake from aqueous solution.

13.
J Org Chem ; 84(18): 11581-11595, 2019 09 20.
Artigo em Inglês | MEDLINE | ID: mdl-31433653

RESUMO

A new one-pot, transition-metal, acid/base-free domino process is developed for the regioselective synthesis of 1,2,4-trisubstituted pyrroles. The process involves 1,3-dipolar cycloaddition of unsymmetrical azomethine ylide resulting from the thermal C-C bond cleavage of unactivated aziridines with ß-bromo-ß-nitrostyrene, followed by a cascade of elimination and aromatization reaction sequence to preferentially furnish 1,2,4-trisubstituted pyrroles instead of the expected 1,2,3-trisubstituted pyrroles, in good to excellent yields. Further, the application of the methodology for the formal synthesis of ningalin B is delineated.

14.
J Org Chem ; 84(18): 11596-11603, 2019 09 20.
Artigo em Inglês | MEDLINE | ID: mdl-31433662

RESUMO

Short and scalable total syntheses of lamellarin G trimethyl ether, lamellarin D trimethyl ether, lamellarin H, lamellarin η, dihydrolamellarin η, and lamellarin U have been realized in four to six linear steps with an overall yield of ≤22%. Highlights of the synthesis include single-step access to the central 1,2,4-trisubstituted pyrrole core in a highly regioselective manner via a one-pot [3+2] cycloaddition/elimination/aromatization sequence-based domino process. Subsequent, palladium-mediated double C-H oxidative coupling in a single-pot operation provides access to the pentacyclic coumarin-fused pyrrolo-dihydroisoquinoline core present in lamellarins.


Assuntos
Alcaloides/síntese química , Produtos Biológicos/síntese química , Cumarínicos/síntese química , Compostos Heterocíclicos de 4 ou mais Anéis/síntese química , Isoquinolinas/síntese química , Pirróis/química , Alcaloides/química , Produtos Biológicos/química , Cumarínicos/química , Reação de Cicloadição , Compostos Heterocíclicos de 4 ou mais Anéis/química , Isoquinolinas/química , Estrutura Molecular
15.
Org Biomol Chem ; 17(28): 6831-6842, 2019 07 17.
Artigo em Inglês | MEDLINE | ID: mdl-31250873

RESUMO

A simple and general approach towards the total syntheses of several iridolactones such as (±)-boschnialactone, (±)-7-epi-boschnialactone, (±)-teucriumlactone, (±)-iridomyrmecin, (±)-isoboonein, (±)-7-epi-argyol, (±)-scabrol A, (±)-7-epi-scabrol A, and (±)-patriscabrol as well as the putative structure of scholarein A is delineated. The synthetic strategy features a diastereoselective intramolecular Pauson-Khand reaction (IPKR) to construct the iridoid framework followed by some strategic synthetic manipulations to access the targeted monoterpenes including those having diverse oxy-functionalization patterns and with 3-5 contiguous stereogenic centres in a highly stereocontrolled manner. Also, the present endeavour includes the first total synthesis of scabrol A.


Assuntos
Alcaloides Indólicos/síntese química , Iridoides/síntese química , Lactonas/síntese química , Alcaloides Indólicos/química , Iridoides/química , Lactonas/química , Conformação Molecular , Soluções , Estereoisomerismo
16.
Bioprocess Biosyst Eng ; 38(12): 2397-416, 2015 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-26458821

RESUMO

The present study explores the reducing and capping potentials of aqueous Raphanus sativus root extract for the synthesis of silver nanomaterials for the first time in the absence and presence of two stabilizers, namely, water-soluble starch and cetyltrimethylammonium bromide (CTAB). The surface properties of silver nanoparticles (AgNPs) were determined by dynamic light scattering (DLS), transmission electron microscopy (TEM), energy dispersion X-ray spectroscopy (EDX), scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier transform infrared (FT-IR) techniques. The mean size of AgNPs, ranging from 3.2 to 6.0 nm, could be facilely controlled by merely varying the initial [extract], [CTAB], [starch], and [Ag(+)] ions. The agglomeration number, average number of silver atoms per nanoparticle, and changes in the fermi potentials were calculated and discussed. The AgNPs were evaluated for their antimicrobial activities against different pathogenic organisms. The inhibition action was due to the structural changes in the protein cell wall.


Assuntos
Anti-Infecciosos/farmacologia , Nanopartículas Metálicas , Extratos Vegetais/metabolismo , Raphanus/metabolismo , Prata/química , Bactérias/efeitos dos fármacos , Fungos/efeitos dos fármacos , Testes de Sensibilidade Microbiana , Microscopia Eletrônica de Varredura , Microscopia Eletrônica de Transmissão , Espectrometria por Raios X , Espectroscopia de Infravermelho com Transformada de Fourier , Difração de Raios X
17.
Angew Chem Int Ed Engl ; 54(32): 9203-8, 2015 Aug 03.
Artigo em Inglês | MEDLINE | ID: mdl-26096055

RESUMO

The total synthesis and structural revision of antibiotic CJ-16,264 is described. Starting with citronellal, the quest for the target molecule featured a novel bis-transannular Diels-Alder reaction that casted stereoselectively the decalin system and included the synthesis of six isomers before demystification of its true structure.


Assuntos
Antibacterianos/síntese química , Lactonas/síntese química , Pirazóis/síntese química , Produtos Biológicos/síntese química , Produtos Biológicos/química , Cristalografia por Raios X , Reação de Cicloadição , Lactonas/química , Conformação Molecular , Naftalenos/química , Pirazóis/química , Estereoisomerismo
18.
Spectrochim Acta A Mol Biomol Spectrosc ; 149: 889-97, 2015 Oct 05.
Artigo em Inglês | MEDLINE | ID: mdl-26004098

RESUMO

In this paper we report the UV-visible and transmission electron microscopy (TEM) evidence to the formation of stable yellow-orange colored complex, which is attributed to the formation of ion-pair between sub-aggregates of cetyltrimethylammonium bromide (CTAB) and gold at room temperature. The position of wavelength maxima (λmax) and shape of the spectra strongly depends on the reaction conditions, i.e., [HAuCl4] and [CTAB]. As the reaction proceeds, typical two bands (one peak and one shoulder) at ca. 409 nm and 470 nm appears and the intensities increase with the time. TEM photographs indicate that the gold-CTA complex consist of aggregated nano-flower like gold with particle size range ca. 40-60 nm. N-(4-hydroxyphenyl)ethanamide (paracetamol) was used to the reduction of resulting gold-CTA complex which leads to the formation of beautiful nano-flower, branched-leaves, and bird-plume like AuNPs. Paracetamol concentrations have marked influence on the morphology (shape, size and the size distribution) and nature of the surface resonance plasmon band of AuNPs whereas [CTAB] have no impact on their spectra. Suitable mechanism have been proposed and discussed to the AuNPs formation.

19.
Environ Sci Pollut Res Int ; 21(5): 3218-29, 2014 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-24203255

RESUMO

Bagasse fly ash (BFA, a sugar industrial waste) was used as low-cost adsorbent for the uptake of arsenate and arsenite species from water. The optimum conditions for the removal of both species of arsenic were as follows: pH 7.0, concentration 50.0 µg/L, contact time 50.0 min, adsorbent dose 3.0 g/L, and temperature 20.0 °C, with 95.0 and 89.5 % removal of arsenate and arsenite, respectively. The Langmuir, Freundlich, Temkin, and Dubinin-Radushkevich adsorption isotherms were used to analyze the results. The results of these models indicated single-layer uniform adsorption on heterogeneous surface. Thermodynamic parameters, i.e., ΔG°, ΔH°, and ΔS°, were also calculated. At 20.0 to 30.0 °C, the values of ΔG° lie in the range of -4,722.75 to -4,878.82 and -4,308.80 to -4,451.73 while the values of ΔH° and ΔS° were -149.90 and -121.07, and 15.61 and 14.29 for arsenate and arsenite, respectively, indicating that adsorption is spontaneous and exothermic. Pseudo-first-order kinetics was followed. In column experiments, the adsorption decreased as the flow rate increased with the maximum removal of 98.9 and 95.6 % for arsenate and arsenite, respectively. The bed depth service time and Yoon and Nelson models were used to analyze the experimental data. The adsorption capacity (N o) of BFA on column was 3.65 and 2.98 mg/cm(3) for arsenate and arsenite, respectively. The developed system for the removal of arsenate and arsenite species is economic, rapid, and capable of working under natural conditions. It may be used for the removal of arsenic species from any contaminated water resources.


Assuntos
Arseniatos/química , Arsenitos/química , Celulose , Poluentes Químicos da Água/química , Purificação da Água/métodos , Adsorção , Concentração de Íons de Hidrogênio , Resíduos Industriais , Cinética , Saccharum , Temperatura , Termodinâmica
20.
Environ Sci Pollut Res Int ; 20(8): 5425-40, 2013 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-23423866

RESUMO

Arsenic contamination of groundwater is a major threat to human beings globally. Among various methods available for arsenic removal, adsorption is fast, inexpensive, selective, accurate, reproducible and eco-friendly in nature. The present paper describes removal of arsenate from water on zirconium oxide-coated sand (novel adsorbent). In the present work, zirconium oxide-coated sand was prepared and characterised by infrared and X-ray diffraction techniques. Batch experiments were performed to optimise different adsorption parameters such as initial arsenate concentration (100-1,000 µg/L), dose (1-8 g/L), pH of the solution (2-14), contact time (15-150 min.), and temperature (20, 30, 35 and 40 °C). The experimental data were analysed by Langmuir, Freundlich, Temkin and Dubinin-Radushkevich isotherm models. Furthermore, thermodynamic and kinetic parameters were evaluated to know the mode of adsorption between ZrOCMS and As(V). The maximum removal of arsenic, 97 %, was achieved at initial arsenic concentration of 200 µg/L, after 75 min at dosage of 5.0 g/L, pH 7.0 and 27 ± 2 °C. For 600 µg/L concentration, the maximum Langmuir monolayer adsorption capacity was found to be 270 µg/g at 35 °C. Kinetic modelling data indicated that adsorption process followed pseudo-second-order kinetics. The mechanism is controlled by liquid film diffusion model. Thermodynamic parameter, ΔH°, was -57.782, while the values of ΔG° were -9.460, -12.183, -13.343 and -13.905 kJ/mol at 20, 30, 35 and 40 °C, respectively, suggesting exothermic and spontaneous nature of the process. The change in entropy, ΔS°= -0.23 kJ/mol indicated that the entropy decreased due to adsorption of arsenate ion onto the solid adsorbent. The results indicated that the reported zirconium oxide-coated marine sand (ZrOCMS) was good adsorbent with 97 % removal capacity at 200 µg/L concentration. It is interesting to note that the permissible limit of arsenic as per World Health Organization is 10 µg/L, and in real situation, this low concentration can be achieved through this adsorbent. Besides, the adsorption capacity showed that this adsorbent may be used for the removal of arsenic from any natural water resource.


Assuntos
Arsênio/química , Dióxido de Silício/química , Poluentes Químicos da Água/química , Purificação da Água/métodos , Zircônio/química , Adsorção , Concentração de Íons de Hidrogênio , Cinética , Temperatura , Termodinâmica
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