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1.
Environ Res ; 258: 119471, 2024 Jun 22.
Artigo em Inglês | MEDLINE | ID: mdl-38914256

RESUMO

Organic dye and nitrophenol pollution from textiles and other industries present a substantial risk to people and aquatic life. One of the most essential remediation techniques is photocatalysis, which uses the strength of visible light to decolorize water. The present study reports Canthium Parviflorum (CNP) leaf extract utilization as an effective bio-reductant for green synthesis of Au NPs. A simple, eco-friendly process with low reaction time and temperature was adopted to synthesize CNP extract-mediated Au-NPs (CNP-AuNPs). The prepared AuNPs characterization involving X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), energy-dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron microscopy (XPS) surface area analysis, ultraviolet-visible spectroscopy (UV-Vis). XRD results showed that the cubic-structured AuNPs had a crystallite size of 14.12 nm. Assessment of organic dyes performance in degrading brilliant green (BTG) and amido black 10B (AMB) under visible light irradiation highlights an impressive 83.25% and 86% degradation efficiency within 120 min, accompanied by a kinetic rate constant dyes was found to be 0.0828 min⁻1, BTG, and 0.0123 min⁻1, Furthermore, the reduction of 4-nitrophenol by NaBH4 using CNP-AuNPs as a catalyst demonstrated good catalytic performance and rapid degradation at 89.4%. and rate constant 0.099 min-1 followed pseudo-first-order. The LC-MS analysis identified various intermediates during the degradation of the CR dye. Radical trapping experiments suggest that photogenerated free electrons and hydroxyl radicals are crucial for degrading the amido black 10B dye The AuNPs influenced the significant factors responsible for the photocatalytic activity, such as the increase in range of absorbance, increased e- and h+ pair separation, improvement in the charge transfer process, and active site formation, which significantly enhanced the process of degradation. We found that the CNP-AuNPs could effectively remove dyes and nitrophenol from industrial wastewater.

4.
Mikrochim Acta ; 191(4): 182, 2024 03 07.
Artigo em Inglês | MEDLINE | ID: mdl-38451377

RESUMO

The rapid fabrication is described of binary electrocatalyst based on a highly porous metal-organic framework with zirconium metal core (Zr-MOF) decorated over the graphitic carbon nitride (g-C3N4) nanosheets via facile ultrasonication method. It is used for the robust determination of antipsychotic drug chlorpromazine (CLP) from environmental samples. The electrochemical behaviour of 2D Zr-MOF@g-C3N4 was characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) studies. The crystalline and porous nature of the composite was characterized by XRD and SEM analysis. The functional groups and surface characteristics were investigated by FT-IR, Raman and XPS. The major electrochemical properties of the Zr-MOF@g-C3N4 composite towards CLP detection were analyzed by CV, chronocoulometric (CC), chronoamperometric (CA) and differential pulse voltammetry (DPV) techniques. The composite exhibits a low detection limit (LOD) of 2.45 nM with a linear range of 0.02 to 2.99 µM and attractive sensitivity for CLP. The sensor system shows higher selectivity towards the possible interferences of CLP drug and exhibits better repeatability and stability. Finally, the fabricated sensor system shows a high recovery range varying from 96.2 to 98.9% towards the real samples. The proposed electrochemical probe might be a promising alternative to the prevailing diagnostic tools for the detection of CLP.


Assuntos
Antipsicóticos , Clorpromazina , Espectroscopia de Infravermelho com Transformada de Fourier , Espectroscopia Dielétrica , Eletrodos
5.
RSC Adv ; 14(3): 1655-1664, 2024 Jan 03.
Artigo em Inglês | MEDLINE | ID: mdl-38187454

RESUMO

The development of electrode materials with extraordinary energy densities or high power densities has experienced a spectacular upsurge because of significant advances in energy storage technology. In recent years, the family of metal-organic frameworks (MOFs) has become an essential contender for electrode materials. Herein, two cobalt-based MOFs are synthesized with distinct linkers named 1,2,4,5-benzene-tetra-carboxylic acid (BTCA) and 1,2,3,4-cyclopentane-tetracarboxylic acid (CPTC). Investigations have been rigorously conducted to fully understand the effect of linkers on the electrochemical properties of Co-based MOFs. The best sample among the MOFs was used with activated carbon to create a battery-supercapacitor hybrid device. Due to its noteworthy results, specific capacity (100.3 C g-1), energy density (23 W h kg-1), power density (3400 W kg-1) and with the lowest ESR value of 0.4 Ω as well as its 95.4% capacity retention, the fabricated hybrid device was discovered to be very appealing for applications demanding energy storage. An approach for evaluating battery-supercapacitors was employed by quantifying the capacitive and diffusive contributions using Dunn's model to reflect the bulk and surface processes occurring during charge storage. This study fills the gap between supercapacitors and batteries, as well as providing a roadmap for creating a new generation of energy storage technologies with improved features.

6.
Heliyon ; 9(11): e21314, 2023 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-38027916

RESUMO

Metal Organic framework (MOF) has been a class of great interest during the past few years owing to its decidedly applicative, easily synthesized and improved characteristics. Ca-BTC MOF is synthesized by Hydrothermal technique and reported for the first time. Its structural morphology was analyzed using XRD, SEM, and EDS, showing the tetragonal crystal structure having grain size of 24.92 nm and purity of sample respectively. FTIR, Raman Spectroscopy ensures the metal organic framework between Calcium and the tri-carboxylic group. Photoluminescence measures the energy gap of 3.792 eV, showing approximately the semiconducting behavior of synthesized material. Zeta potential having value of -13.5 mV confirms the instability having good microbial activity and conductivity i.e 0.290 mS/cm which reveals important insights into its electrical properties.

7.
Sci Rep ; 13(1): 14728, 2023 Sep 07.
Artigo em Inglês | MEDLINE | ID: mdl-37679372

RESUMO

This work presents the simple synthesis of a green and novel Palladium based magnetic nanocatalyst with effective catalytic properties and reusability. These heterogeneous catalysts were prepared by the anchoring of Pd(0) on the surface of ZrFe2O4 MNPs coated with a di-substituted adenine (Ade) compound as a green linker. The as-synthesized ZrFe2O4@SiO2@Ade-Pd MNPs were methodically characterized over different physicochemical measures like VSM, EDX, Map, SEM, TEM, ICP, and FT-IR analysis. The catalytic activity of ZrFe2O4@SiO2@Ade-Pd was carefully examined for the room-temperature Carbon-Carbon coupling reaction in acetonitrile as a solvent. It is worth noting that the synthesized solid catalyst can be easily recovered with a bar magnet and reused for five cycles without decrease of catalytic activity.

8.
J Chromatogr A ; 1707: 464326, 2023 Sep 27.
Artigo em Inglês | MEDLINE | ID: mdl-37639846

RESUMO

Preconcentration for on-site detection or subsequent determination is a promising technique for selective sensing explosive markers at low concentrations. Here, we report divinylbenzene monolithic polymer in its blank form (neat-DVB) and as a composite incorporated with sodalite topology zeolite-like metal-organic frameworks (3-ZMOF@DVB), as a sensitive, selective, and cost-effective porous preconcentrator for aliphatic nitroalkanes in the vapor phase as explosive markers at infinite dilution. The developed materials were fabricated as 18 cm gas chromatography (GC) monolithic capillary columns to study their separation performance of nitroalkane mixture and the subsequent physicochemical study of adsorption using the inverse gas chromatography (IGC) technique. A strong preconcentration effect was indicated by a specific retention volume adsorption/desorption ratio equal to 3 for nitromethane on the neat-DVB monolith host-guest interaction, and a 14% higher ratio was observed using the 3-ZMOF@DVB monolithic composite despite the low percentage of 0.7 wt.% of sod-ZMOF added. Furthermore, Incorporating ZMOF resulted in a higher percentage of micropores, increasing the degree of freedom more than bringing stronger adsorption and entropic-driven interaction more than enthalpic. The specific free energy of adsorption (ΔGS) values increased for polar probes and nitroalkanes, denoting that adding ZMOFs earned the DVB monolithic matrix a more specific character. Afterward, Lewis acid-base properties were calculated, estimating the electron acceptor (KA) and electron donor (KB) constants. The neat-DVB was found to have a Lewis basic character with KB/KA = 7.71, and the 3-ZMOF@DVB had a less Lewis basic character with KB/KA = 3.82. An increased electron-accepting nature can be directly related to incorporating sod-ZMOF into the DVB monolithic matrix. This work considers the initial step in presenting a portable explosives detector or preconcentrating explosive markers trace prior to more sophisticated analysis. Additionally, the IGC technique allows for understanding the factors that led to the superior adsorption of nitroalkanes for the developed materials.


Assuntos
Substâncias Explosivas , Estruturas Metalorgânicas , Zeolitas , Polímeros , Alcanos , Bases de Lewis
9.
J Chromatogr A ; 1694: 463922, 2023 Apr 12.
Artigo em Inglês | MEDLINE | ID: mdl-36931139

RESUMO

Organic monolithic columns are mainly used to separate macromolecules; however, many attempts to extend their performance toward small molecules were examined by incorporating micro- and nanoparticles. The incorporation technique enabled utilizing organic monoliths in gas chromatography (GC) for small molecules, which are still scarce. Here, we prepared a composite matrix of capillary monolithic columns of a zeolite-like metal-organic framework with a sodalite topology (sod-ZMOF) and Divinylbenzene polymer (DVB) for GC separations under 0.5 MPa. Relatively short DVB monolithic columns (18 cm long × 0.25 mm i.d.) incorporated with a tiny amount of sod-ZMOF nanoparticles (0.7 and 1.17 wt%) with an average particle size of 225 nm were successfully fabricated and used to separate linear alkanes and polar probes mixtures with increasing resolution up to 3.7 and 5.1 times, respectively, compared to a blank DVB monolithic column. A high-performance separation of linear alkanes series mixture (methane to decane) was exhibited in less than 2 min. McReynolds constants revealed that sod-ZMOF provided the composite monolith with a nonpolar character yielding a negative average polarity value smaller than the standard squalene column. An Excellent retention time of pentane and octane day-to-day reproducibility was achieved during 16 days and over more than 500 runs with RSD% of 2.25% and 3.3% using a composite monolithic column with 5 mg mL-1 sod-ZMOF (5-ZMOF@DVB). In addition, a qualitative determination of the gas mixture content of three commercially available Lighter gas cartridges was performed via the 5-ZMOF@DVB column. Finally, successfully separating an azeotropic freon mixture of difluoromethane (R-32) and pentafluoroethane (R-125) was achieved with a selectivity of up to 4.84. A further thermodynamic study related the preferential adsorption of R-125 to entropic factors rather than enthalpic while trapping inside ZMOF pores. This work sheds light on utilizing the infinite diversity of MOFs and combining their properties with high permeability and easily fabricated organic monoliths for GC separations of light molecules and gasses. Furthermore, the study highlights the role of GC as an easy and fast approach for the preliminary evaluation of the separation efficiency of porous polymers.


Assuntos
Fluorocarbonos , Estruturas Metalorgânicas , Zeolitas , Polímeros/química , Reprodutibilidade dos Testes , Alcanos/análise , Fluorocarbonos/análise
10.
J Chromatogr A ; 1690: 463695, 2023 Feb 08.
Artigo em Inglês | MEDLINE | ID: mdl-36682103

RESUMO

This work relates to the preparation of novel and promising stationary phases containing inorganic-organic composites for capillary liquid and gas chromatography. A naturally occurring montmorillonite was introduced to polymethacrylate monoliths, then used under different conditions of GC and HPLC at the same time. The performance of the columns was evaluated for the separation of alkane and alkylbenzene series in GC and capillary HPLC, respectively. While the bare monoliths failed to separate the model analytes, montmorillonite-based polymethacrylate allowed a full separation of the mixtures with Rs≥1.42. The columns were applied for the determination of myrcene and limonene isomers in the peel extracts of some fruits using GC, and for the analysis of active ingredients including aspirin, vitamin-C, caffeine, and ibuprofen extracted from common drugs using capillary HPLC. In GC, fast separation was achieved in 1.0 min with Rs of 6.53. The columns exhibited the best efficiency for myrcene with 20,900 plates/m. Using the capillary HPLC columns, the active ingredients were resolved in 10 min with Rs≥5.72. The efficiency values located between 12,800-21,700 plates/m in all cases. The developed methods were found to be linear in the range of 0.10-10.0 and 0.20-180 µg/mL for GC and HPLC, respectively. In comparison with commercial columns, the results in GC methods reveal that, despite their much shorter length, the prepared columns proved a faster separation with higher efficiency and comparable detection limits and chromatographic resolution. The prepared HPLC capillaries exposed lower run times and detection limits with comparable efficiency and resolution, and consume fewer samples and mobile phase solvents. The results demonstrate that the montmorillonite-based polymethacrylate composites are applicable as stationary phases for routine analysis and quality control of important fields such as food and pharmaceutical samples.


Assuntos
Bentonita , Capilares , Cromatografia Gasosa/métodos , Preparações Farmacêuticas
11.
J Am Chem Soc ; 144(43): 19813-19824, 2022 Nov 02.
Artigo em Inglês | MEDLINE | ID: mdl-36265086

RESUMO

Two-dimensional (2D) covalent organic frameworks (COFs) are composed of structurally precise, permanently porous, layered macromolecular sheets, which are traditionally synthesized as polycrystalline solids with crystalline domain lengths smaller than 100 nm. Here, we polymerize imine-linked 2D COFs as suspensions of faceted single crystals in as little as 5 min at moderate temperature and ambient pressure. Single crystals of two imine-linked 2D COFs were prepared, consisting of a rhombic 2D COF (TAPPy-PDA) and a hexagonal 2D COF (TAPB-DMPDA). The sizes of TAPPy-PDA and TAPB-DMPDA crystals were tuned from 720 nm to 4 µm and 450 nm to 20 µm in width, respectively. High-resolution transmission electron microscopy revealed that the COF crystals consist of layered, 2D polymers comprising single-crystalline domains. Continuous rotation electron diffraction resolved the unit cell and crystal structure of both COFs, which are single-crystalline in the a-b plane but disordered in the stacking c dimension. Single crystals of both COFs were incorporated into gas chromatography separation columns and exhibited unusual selective retention of cyclohexane over benzene, with single-crystalline TAPPy-PDA significantly outperforming single-crystalline TAPB-DMPDA. Polycrystalline TAPPy-PDA exhibited no separation, while polycrystalline TAPB-DMPDA exhibited poor separation and the opposite order of elution, retaining benzene more than cyclohexane, indicating the importance of improved material quality for COFs to exhibit properties that derive from their precise, crystalline structures. This work represents the first example of synthesizing imine-linked 2D COF single crystals at ambient pressure and short reaction times and demonstrates the promise of high-quality COFs for molecular separations.

12.
Chirality ; 34(10): 1383-1388, 2022 10.
Artigo em Inglês | MEDLINE | ID: mdl-35735121

RESUMO

WHO is searching most active antibiotics due to the bacterial resistance problem. The activities of the racemic antibiotics may be augment by preparing optically active antibiotics by the chiral separation. Chiral separation of potential antibiotics such as cefotaxime and ofloxacin was studied using amylose-based packing chiral stationary phases (CSPs) such as Chiralpak IA and Chiralpak IG. Supercritical fluid chromatography (SFC) was employed to carry out this study. Both immobilized CSPs such as Chiralpak IA and IG have sown remarkable selectivity for the reported drugs by using SFC. The values of retention factor (k) for ofloxacin enantiomers were 9.63 and 11.81, followed by 2.94 and 5.96 for cefotaxime enantiomers. The values of separation factor (α) for both the reported drugs were 1.22 and 2.03, respectively Similarly, the values of resolution factor (Rs) for both the enantio-selective drugs were 1.49 and 2.06, separately and respectively. The chiral recognition mechanism was developed and it was observed that the π-π interactions are playing a major role. The developed method is effective, reproducible, eco-friendly, and may be used to discriminate the enantiomers of the reported drugs in any sample.


Assuntos
Cromatografia com Fluido Supercrítico , Antibacterianos , Cefotaxima , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia com Fluido Supercrítico/métodos , Ofloxacino , Estereoisomerismo
13.
Chirality ; 34(6): 848-855, 2022 06.
Artigo em Inglês | MEDLINE | ID: mdl-35297109

RESUMO

Chiral separation of ß-blockers is performed by utilizing the supercritical fluid chromatographic method. The chiral columns utilized were Chiralpak IG and Chiralpak IBN-5. The finest mobile phase was CO2 -0.2% TEA in methanol (60:40). The values atenolol enantiomers retention factors were 6.39 and 8.98. These values for propranolol enantiomers were 3.39 and 4.06. These values for betaxolol enantiomers were 4.08 and 4.68. The separation and resolution factor values for atenolol, propranolol, and betaxolol were 1.41 and 3.33, 1.19 and 2.23, and 1.15 and 1.87, separately and respectively. By comparison, it was observed that Chiralpak IG column is better than Chiralpak IBN-5 column. Supercritical fluid chromatography has been found as the best analytical technique due to its high speed, being eco-friendly, and being economic. The various most probable interactions responsible for the chiral resolution are hydrogen bonding, dipole-dipole interactions, steric effect, and π-π interactions. The reported methods are effective, efficient, and reproducible and may be used to separate and identify atenolol, propranolol, and betaxolol in any unknown samples.


Assuntos
Cromatografia com Fluido Supercrítico , Antagonistas Adrenérgicos beta , Atenolol , Betaxolol , Cromatografia com Fluido Supercrítico/métodos , Propranolol , Estereoisomerismo
14.
J Chromatogr A ; 1443: 233-40, 2016 Apr 22.
Artigo em Inglês | MEDLINE | ID: mdl-26997561

RESUMO

UNLABELLED: Thermodynamic characterization of butyl methacrylate-co-ethylene dimethacrylate neat monolith and zeolitic imidazolate framework-8 incorporated with butyl methacrylate-co-ethylene dimethacrylate composite monolith were studied using inverse gas chromatography at infinite dilution under 1MPa column pressure and various column temperatures. The free energy of adsorption (ΔGA), enthalpy of adsorption (ΔHA) and entropy of adsorption (ΔSA) were determined using a series of n-alkanes. The dispersive component of surface energy (γS(D)) was estimated by Dorris-Gray and Schultz et al. METHODS: The composite monolith showed a more energetic surface than the neat monolith. The acidic, KA, and basic, KD, parameters for both materials were estimated using a group of polar probes. A basic character was concluded with more basic behavior for the neat monolith. Flory-Huggins parameter, χ, was taken as a measure of miscibility between the probes with the low molecular weight and the high molecular weight monolith. Inverse gas chromatography provides a better understanding of the role of incorporated zeolitic imidazolate framework (ZIF-8) into the polymer matrix in its monolithic form.


Assuntos
Técnicas de Química Analítica , Cromatografia Gasosa , Imidazóis/análise , Metacrilatos/análise , Adsorção , Alcanos/química , Imidazóis/química , Metacrilatos/química , Polímeros/química , Termodinâmica
15.
J Sep Sci ; 39(5): 880-8, 2016 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-26711438

RESUMO

A monolithic capillary column containing a composite of metal-organic framework MIL-53(Al) incorporated into hexyl methacrylate-co-ethylene dimethacrylate was prepared to enhance the separation of mixtures of small aromatic compounds by using capillary liquid chromatography. The addition of 10 mg/mL MIL-53(Al) microparticles increased the micropore content in the monolithic matrix and increased the Brunauer-Emmett-Teller surface area from 26.92 to 85.12 m(2) /g. The presence of 1,4-benzenedicarboxylate moieties within the structure of MIL-53(Al) as an organic linker greatly influenced the separation of aromatic mixtures through π-π interactions. High-resolution separation was obtained for a series of alkylbenzenes (with resolution factors in the range 0.96-1.75) in less than 8 min, with 14 710 plates/m efficiency for propylbenzene, using a binary polar mobile phase of water/acetonitrile in isocratic mode. A reversed-phase separation mechanism was indicated by the increased retention factor and resolution as the water percentage in the mobile phase increased. A stability study on the composite column showed excellent mechanical stability under various conditions. The higher resolution and faster separation observed at increased temperature indicated an exothermic separation, whereas the negative values for the free energy change of transfer indicated a spontaneous process.

16.
J Chromatogr A ; 1406: 299-306, 2015 Aug 07.
Artigo em Inglês | MEDLINE | ID: mdl-26141277

RESUMO

A composite zeolitic imidazolate framework-8 (ZIF-8) with a butyl methacrylate-co-ethylene dimethacrylate (BuMA-co-EDMA) monolithic capillary column (33.5cm long×250µm i.d.) was fabricated to enhance the separation efficiency of methacrylate monoliths toward small molecules using conventional low-pressure gas chromatography in comparison with a neat butyl methacrylate-co-ethylene dimethacrylate (BuMA-co-EDMA) monolithic capillary column (33.5cm long×250µm i.d.). The addition of 10mgmL(-1) ZIF-8 micro-particles increased the BET surface area of BuMA-co-EDMA by 3.4-fold. A fast separation of five linear alkanes in 36s with high resolution (Rs≥1.3) was performed using temperature program. Isothermal separation of the same sample also showed a high efficiency (3315platesm(-1) for octane) at 0.89min. Moreover, the column was able to separate skeletal isomers, such as iso-octane/octane and 2-methyl octane/nonane. In addition, an iso-butane/iso-butylene gas mixture was separated at ambient temperature. Comparison with an open tubular TR-5MS column (30m long×250µm i.d.) revealed the superiority of the composite column in separating the five-membered linear alkane mixture with 4-5 times increase in efficiency and a total separation time of 0.89min instead of 4.67min. A paint thinner sample was fully separated using the composite column in 2.43min with a good resolution (Rs≥0.89). The perfect combination between the polymeric monolith, with its high permeability, and ZIF-8, with its high surface area and flexible 0.34nm pore openings, led to the fast separation of small molecules with high efficiency and opened a new horizon in GC applications.


Assuntos
Cromatografia Gasosa/instrumentação , Imidazóis/química , Alcanos/química , Isomerismo , Metacrilatos/química , Compostos Orgânicos/química
17.
J Chromatogr A ; 1348: 1-16, 2014 Jun 27.
Artigo em Inglês | MEDLINE | ID: mdl-24845827

RESUMO

Metal-organic frameworks (MOFs) emerged approximately two decades ago and are the youngest class of porous materials. Despite their short existence, MOFs are finding applications in a variety of fields because of their outstanding chemical and physical properties. This review article focuses on the applications of MOFs in chromatography, including high-performance liquid chromatography (HPLC), gas chromatography (GC), and other chromatographic techniques. The use of MOFs in chromatography has already had a significant impact; however, the utilisation of MOFs in chromatography is still less common than other applications, and the number of MOF materials explored in chromatography applications is limited.


Assuntos
Cromatografia/instrumentação , Metais/química , Cromatografia Gasosa/instrumentação , Cromatografia Líquida de Alta Pressão/instrumentação , Porosidade
18.
J Chromatogr Sci ; 52(3): 201-10, 2014 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-23424040

RESUMO

This paper describes the comprehensive fabrication of monolithic materials for use as stationary phases in capillary liquid chromatography. Several columns were synthesized in the confines of 320 µm i.d. fused-silica capillaries by single-step in situ copolymerization of benzyl methacrylate and ethylene dimethacrylate (EDMA). The polymerization procedure was optimized by varying the reaction time within the range of 0.5-20 h, and by changing the composition contents of the polymeric mixture. The EDMA content showed a predominant influence on the characteristics of the columns and hence, on their chromatographic properties. The optimum value of the thermal initiator corresponded to 5 mg/mL. Changes of the porous, hydrodynamic properties and morphology of the prepared columns were thoroughly investigated and characterized. Different solvents were used as the mobile phase to demonstrate that the resulting monoliths exhibited good permeability and mechanical stability, whereas swelling and shrinking behaviors were observed and discussed. The efficiency and performance toward different sets of analytes were obtained; mixtures of aromatic hydrocarbons and phenolic compounds were successfully separated and evaluated, and adding tetrahydrofuran to the mobile phase showed improvement in both resolution and peak shapes. The characteristics of the columns were also checked in terms of repeatability and reproducibility.

19.
J Chromatogr A ; 1301: 200-8, 2013 Aug 02.
Artigo em Inglês | MEDLINE | ID: mdl-23806355

RESUMO

Gas chromatography (GC) is considered the least common application of both polymer and silica-based monolithic columns. This study describes the fabrication of alkyl methacrylate monolithic materials for use as stationary phases in capillary gas chromatography. Following the deactivation of the capillary surface with 3-(trimethoxysilyl)propyl methacrylate (TMSM), the monoliths were formed by the co-polymerization of either hexyl methacrylate (HMA) or lauryl methacrylate (LMA) with different percentage of ethylene glycol dimethacrylate (EDMA) in presence of an initiator (azobisisobutyronitrile, AIBN) and a mixture of porogens include 1-propanol, 1,4-butanediol and water. The monoliths were prepared in 500mm length capillaries possessing inner diameters of 250µm. The efficiencies of the monolithic columns for low molecular weight compounds significantly improved as the percentage of crosslinker was increased, because of the greater proportion of pores less than 50nm. The columns containing lower percentages of crosslinker were able to rapidly separate a series of 8 alkane members in 0.7min, but the separation was less efficient for the light alkanes. Columns prepared with the lauryl methacrylate monomer yielded a different morphology for the monolith-interconnected channels. The channels were more branched, which increased the separation time, and unlike the other columns, allowed for temperature programming.


Assuntos
Cromatografia Gasosa/instrumentação , Metacrilatos/química , Alcanos/análise , Alcanos/isolamento & purificação , Cromatografia Gasosa/métodos , Gasolina/análise , Hidrodinâmica , Modelos Químicos , Porosidade
20.
PLoS One ; 8(3): e59177, 2013.
Artigo em Inglês | MEDLINE | ID: mdl-23555627

RESUMO

The present study was undertaken to investigate the protective effect of the filamentous cyanobacterium Spirulina platensis (S. platensis) on mercury (II) chloride (HgCl(2))-induced oxidative damages and histopathological alterations in the testis of Wistar albino rats. The animals were divided into four equal groups, i) control, ii) HgCl(2), iii) S. platensis and iv) combination of HgCl(2)+S. platensis. Oxidative stress, induced by a single dose of HgCl(2) (5 mg/kg, bw; subcutaneously, s.c.), substantially decreased (P<0.01) the activity level of testicular key enzymatic antioxidant biomarkers (superoxide dismutase, SOD; catalase, CAT and glutathione peroxidase, GPx), oxidative stress makers (blood hydroperoxide; testicular reduced glutathione, GSH and malondialdehyde, MDA), and testicular mercury levels. Moreover, HgCl(2) administration resulted in a significant (P<0.01) increase in the number of sperms with abnormal morphology and decrease in epididymal sperm count, motility, plasma testosterone level and testicular cholesterol. Furthermore, HgCl(2) exposure induced histopathological changes to the testis including morphological alterations of the seminiferous tubules, and degeneration and dissociation of spermatogenic cells. Notably, oral pretreatment of animals with Spirulina (300 mg/kg, bw) lowered the extent of the observed HgCl(2)-mediated toxicity, whereby significantly reducing the resulting lipid peroxidation products, mercury accumulation in the testis, histopathological changes of the testes and spermatozoal abnormalities. In parallel, the pretreatment with Spirulina also completely reverted the observed Hg-Cl(2)-induced inhibition in enzymatic activities of antioxidant biomarkers (SOD, CAT and GPx) back to control levels. The pretreatment of rats with S. platensis significantly recovered the observed HgCl(2)-mediated decrease in the weight of accessory sex organs. Taken together, our findings clearly highlight the role of S. platensis as a protective modulator of HgCl(2)-induced testicular injuries and suggest some therapeutic potential in mammals. Further investigation of therapeutic strategies employing Spirulina against heavy metals toxicity in humans is therefore warranted.


Assuntos
Antioxidantes/farmacologia , Misturas Complexas/farmacologia , Epididimo/efeitos dos fármacos , Cloreto de Mercúrio/toxicidade , Túbulos Seminíferos/efeitos dos fármacos , Espermatozoides/efeitos dos fármacos , Spirulina/química , Animais , Catalase/metabolismo , Epididimo/lesões , Glutationa/metabolismo , Glutationa Peroxidase/metabolismo , Peroxidação de Lipídeos/efeitos dos fármacos , Masculino , Malondialdeído/sangue , Estresse Oxidativo/efeitos dos fármacos , Ratos , Ratos Wistar , Recuperação de Função Fisiológica , Túbulos Seminíferos/lesões , Motilidade dos Espermatozoides/efeitos dos fármacos , Superóxido Dismutase/metabolismo
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