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An efficient strategy utilizing µ-thin layer chromatography coupled with laser ablation inductively coupled plasma mass spectrometry (µ-TLC-LA-ICP-MS) based on an IIP (ion imprinted polymer) was developed for the speciation of inorganic arsenic [As(III) and As(V)]. The characterization of the fabricated IIP was performed applying Fourier-transform infrared spectroscopy (FTIR) and field emission scanning electron microscopy (FESEM). To prepare the thin layer chromatography plate, CaSO4 (as a binder) was incorporated with the IIP. Then, the surface of the TLC plate was swept by LA, which volatilized the species of arsenic from the thin layer chromatography plate which thereafter were introduced into the ICP-MS system. Various effective parameters on isolation efficiency, such as the IIP/CaSO4 mass ratio, mobile phase composition, and pH, were examined. Under optimized conditions, the developed method demonstrated a detection limit of 0.3 µg L-1 with a wide linear dynamic range of 0.2-100 µg L-1, and a relative standard deviation of 3.8. The performance of the developed method was investigated for the isolation of As(III) and As(V) in wastewater (Mouteh, Aghdareh, and Zarmehr mines) and human blood plasma real samples.
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In the present study, we synthesized DABCOnium-based-Brønsted acidic ionic liquid-functionalized magnetic nanoparticles (Fe3O4@(SU-DBC) NPs). Their structure was characterized using various morphological and physicochemical techniques such as SEM, powder-XRD, XPS, FTIR, VSM, and BET. The Fe3O4@(SU-DBC) NPs have remarkable magnetic recovery, extensive colloidal stability, and excellent recyclability. The fabricated ionic liquid-modified magnetic NPs show capability for magnetic dispersive micro-solid-phase extraction (MD-µ-SPE) of trace metals (Cd, Cr, Ni, and Pb) from sunblock cream samples. Micro-sampling flame atomic absorption spectrometry (MS-FAAS) was used to analyze the analytes. For evaluating the simultaneous effects of various parameters on the extraction efficiency, a central composite design was employed. In the method validation, the recoveries ranged from 97.84 to 102.36%, with relative standard deviations of 0.97% to 3.27%. The detection limits of the proposed method ranged between 0.067 and 0.715 µg kg-1. The developed method showed high sensitivity and precision, and stable recovery. Health risks were evaluated using the margin of safety (MoS), hazard quotient (HQ), hazard index (HI), and lifetime cancer risk (LCR). Sunblock creams' MoS, HQ, and HI values were within permissible ranges, but LCR values were higher than permitted.
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In this research, Hydroxyethyl cellulose - graphene oxide HEC-GO and HEC-GO/Fe-Zn mole ratio (2:1) nanocomposite as adsorbents were fabricated by crosslinking ethylene glycol dimethacrylate (EGDMA) to study the thermodynamic, kinetic and isotherm of doxycycline antibiotic adsorption. The morphology and structure of the adsorbents were analyzed by Fourier transform infrared spectroscopy (FT-IR), Field Emission Scanning Electron Microscopy with Energy Dispersive X-Ray Spectroscopy (FE-SEM- EDX), and Transmission electron microscopy (TEM). The adsorption behavior of doxycycline (DOX) was studied with different parameters including doxycycline concentration, pH, the dose of adsorbent (HEC-GO and HEC-GO/Fe-Zn, mole ratio (2:1)), contact time, and temperature. The optimal conditions for the removal of DOX are pH = 3.0, contact time 100 min, and 20 min for HEC-GO and HEC-GO/Fe-Zn mole ratio (2:1). The removal percentage for HEC-GO and HEC-GO/Fe-Zn mole ratio (2:1) was 97% and 95.5%, respectively. Equilibrium adsorption isotherms such as the Langmuir, Freundlich, and Temkin models were analyzed according to the experimental data. Also, four adsorption kinetics were investigated for removing DOX. The Langmuir isotherm and pseudo-second-order kinetic models provided the best fit for experimental data for HEC-GO and HEC-GO/Fe-Zn mole ratio (2:1). Thermodynamic data showed that negative values of Gibbs free energy (ΔG°) and the negative value of enthalpy (ΔH°) of the adsorption process for adsorbents. It means that DOX removal was a spontaneous and exothermic reaction.
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Nanopartículas , Poluentes Químicos da Água , Doxiciclina , Espectroscopia de Infravermelho com Transformada de Fourier , Termodinâmica , Celulose , Zinco , Adsorção , Cinética , Poluentes Químicos da Água/análise , Concentração de Íons de HidrogênioRESUMO
In this project, the quetiapine drug was used as the template for synthesis of a molecular imprinted polymer (MIP). The polymerization approach for preparation of this composite was precipitation, where methacrylic acid (MAA), ethylene glycol dimethacrylate (EGDMA), and 2,2-azobisissobutyronitrile (AIBN) were used as the functional monomer, the cross-linker, and the initiator, respectively. Scanning electron microscopy (SEM) showed that the diameter of the nanoparticles is about 70 nm. The adsorption rates of quetiapine to the MIP host were evaluated at different pHs, and the results showed that the highest adsorption values were obtained at pH = 7. Moreover, the kinetics of the adsorption process was detected to follow the Langmuir isotherm (R2 = 0.9926) and the pseudo-second-order kinetics (R2 = 0.9937). The results confirmed the high capability of the synthesized MIPs as pharmaceutical carriers for quetiapine. Furthermore, the kinetics of the drug release from the MIP follows the Higuchi model at the pHs of 5.8-6.8 and the Korsmeyer-Peppas model at the pHs of 1.2-5. Finally, in light of the density functional theory (DFT)-based quantum chemical descriptors, the polymer-quetiapine drug complex was designed and investigated. The results showed that there is a strong interaction between the host (polymer) and the guest (drug) due to several hydrogen bonds and other intermolecular (polar) interactions.
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A sensitive method based on liquid chromatography combined with a diode array detector was developed and validated to simultaneously determine tamoxifen, and its active metabolites N-desmethyltamoxifen, 4-hydroxytamoxifen, and endoxifen in human plasma samples. The green and sustainable vortex-assisted dispersive liquid-phase microextraction technique based on the natural hydrophobic deep eutectic solvent was used for the extraction and preconcentration of the analytes. Chemometrics and multivariate analysis were used to optimize the independent variables including the type and volume of deep eutectic solvent, extraction time, and ionic strength. Under optimal conditions, calibration curves were linear in a suitable range with the lower limits of quantification (0.8-10.0 µg/L), which covered the relevant concentrations of the analytes in plasma samples for a clinical study. Intra- and interday precision evaluated at three concentrations for the analytes were lower than 8.2 and 12.1%, respectively. Accuracy was in the range of 94.9-104.7%. The applicability of the developed method on human plasma samples illustrated the range 45.1-72.8, 98.4-128.3, 0.9-1.2, and 2.7-6.1 µg/L for tamoxifen, N-desmethyltamoxifen, 4-hydroxytamoxifen, and endoxifen, respectively. The validated method can be effective for the pharmacokinetics, pharmacodynamics, and therapeutic drug monitoring studies of tamoxifen and its main metabolites in biological fluids.
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Neoplasias da Mama , Sobreviventes de Câncer , Microextração em Fase Líquida , Neoplasias da Mama/tratamento farmacológico , Quimiometria , Cromatografia Líquida de Alta Pressão/métodos , Solventes Eutéticos Profundos , Feminino , Humanos , Limite de Detecção , Microextração em Fase Líquida/métodos , Solventes/química , TamoxifenoRESUMO
Gas flow-assisted dispersive liquid-phase microextraction based on deep eutectic solvent was used to determine parabens in personal care products such as mouthwash, lidocaine gel, aloe vera gel, and skin tonic. A homemade extraction device was innovated, in which by passing the stream of gas bubbles through the deep eutectic solvent a thin layer of the extraction phase is coated on the surface of the bubbles. The extraction is finally achieved when the bubbles are going up through the sample. The single-factor experiments and response surface methodology were applied to optimize the independent variables. The linear range of the method was 0.5 to 1000 µg L-1, the coefficient of determination for the goal analytes was higher than 0.9989, the instrumental limit of detections were in the range 0.2-0.3 µg L-1, and the instrumental limit of quantifications were in the range 0.5-1.1 µg L-1, the relative standard deviations were <5.2% for repeatability and <11.2% for intermediate precision, and the enrichment factors were 66 to 87 obtained under the optimized conditions. A spiking approach by means of standard material was used to estimate accuracy. The relative recoveries were in the range 95.8-105.2%. By using mentioned strategies, the organic waste and energy consumption reduced, toxic reagents replaced with safer ones, and operator safety enhanced. Accordingly, these benefits have been simultaneously attained and, the proposed method was one step closer to automation and sustainable analytical chemistry.
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Cosméticos/química , Microextração em Fase Líquida/métodos , Parabenos/análise , Parabenos/isolamento & purificação , Cromatografia Líquida de Alta Pressão , Química Verde , Limite de Detecção , Modelos Lineares , Parabenos/química , Reprodutibilidade dos Testes , Solventes/químicaRESUMO
In the present research, a new biocompatible electrode is proposed as a rapid and direct glucose biosensing technique that improves on the deficiencies of fast clinical devices in laboratory investigations. Nano-ZnO (nanostructured zinc oxide) was sputtered by reactive direct current magnetron sputtering system on a precovered fluorinated tin oxide (FTO) conductive layer. Spin-coated polyvinyl alcohol (PVA) at optimized instrumental deposition conditions was applied to prepare the effective medium for glucose oxidase enzyme (GOx) covalent immobilization through cyanuric chloride (GOx/nano-ZnO/PVA/FTO). The electrochemical behavior of glucose on the fabricated GOx/nano-ZnO/PVA/FTO biosensor was investigated by I-V techniques. In addition, field emission scanning electron microscopy and electrochemical impedance spectroscopy were applied to assess the morphology of the modified electrode surface. The I-V results indicated good sensitivity for glucose detection (0.041 mA per mM) within 0.2-20 mM and the limit of detection was 2.0 µM. We believe that such biodevices have good potential for tracing a number of biocompounds in biological fluids along with excellent accuracy, selectivity, and precise analysis. The fast response time of the fabricated GOx/nano-ZnO/PVA/FTO biosensor (less than 3 s) could allow most types of real-time analysis.
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In this research, an efficient sorbent based on poly(ß-cyclodextrin-ester)-functionalized silica-coated magnetic nanoparticles (MNPs-CDP) was prepared and used for magnetic solid-phase extraction of the malachite green (MG) and crystal violet (CV) from water samples prior to their determination by high-performance liquid chromatography-ultra violet detection (HPLC-UV). The synthesized nanoparticles were characterized by the field emission-scanning electron microscopy (FE-SEM) and Fourier transform infrared spectroscopy (FT-IR). Of course, the factors, which could influence the extraction efficiency like pH, sorbent amount, salt content, extraction time, desorption time, eluent type, and volume and sample volume, were optimized by response surface methodology. Then, for both of MG and CV, good linearity (0.1-200 µg L-1, r2 ≥ 0.99) was achieved under the optimized conditions. The limits of detection (LODs) and the limits of quantification (LOQs), for both of MG and CV, were 0.03 µg L-1 and 0.1 µg L-1, respectively. Precision of the method expressed as the relative standard deviations (RSDs) at concentration level of 100 µg L-1 was 5.6 and 4.2 for MG and CV, respectively. Ultimately, usability of proposed method was investigated by analysis of CV and MG in tap water, fish pond water, and the lake water, and the satisfactory recoveries were obtained in the range of 92-100.5%.
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Violeta Genciana/química , Nanopartículas de Magnetita , Corantes de Rosanilina/química , Extração em Fase Sólida/métodos , Poluentes Químicos da Água/química , Adsorção , Monitoramento Ambiental , Limite de Detecção , Fenômenos Magnéticos , Dióxido de Silício , Espectroscopia de Infravermelho com Transformada de Fourier , beta-CiclodextrinasRESUMO
Due to the vitamin K1 sensitizing potential, the oxidized-isoform of vitamin K1 (vitamin K1 oxide, VKO), has been recently used for treating laser-induced purpura and hyperpigmentation in cosmetics. The objective of this study was to formulate VKO in nanoliposomes by using Box-Behnken experimental design to obtain an optimized formula with higher efficiency. The ratio of phospholipid to cholesterol (PC/CHO ratio), VKO concentration and sonication time in low, medium, and high levels were independent variables, while the percent of VKO entrapment efficiency (EE%) and vesicle size were selected as dependent variables. Optimum desirability was identified and an optimized formulation was prepared, characterized, and selected for in vitro VKO release and ex vivo skin permeation. The PC/CHO ratio showed the greatest effect on both responses (P < 0.0001). This effect was positive on EE%, while a negative effect was shown on vesicle size. The optimized formulation showed controlled drug release of 79.2% through a silicon membrane, and achieved flux of 327.36 ± 22.1 µg/cm2 through human skin after 24 h. So, nanoliposomes were proven as a suitable drug delivery system for topical delivery of VKO.
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Composição de Medicamentos/métodos , Nanopartículas/química , Vitamina K 1/análogos & derivados , Administração Cutânea , Química Farmacêutica , Colesterol/química , Técnicas Cosméticas/efeitos adversos , Técnicas Cosméticas/instrumentação , Preparações de Ação Retardada/administração & dosagem , Preparações de Ação Retardada/farmacocinética , Liberação Controlada de Fármacos , Humanos , Hiperpigmentação/tratamento farmacológico , Hiperpigmentação/etiologia , Lasers/efeitos adversos , Lipossomos , Tamanho da Partícula , Fosfolipídeos/química , Púrpura/tratamento farmacológico , Púrpura/etiologia , Pele/metabolismo , Pele/efeitos da radiação , Absorção Cutânea , Vitamina K 1/administração & dosagem , Vitamina K 1/farmacocinéticaRESUMO
In this study, for the first time, salt-assisted liquid-liquid extraction was performed in a microchannel system. The proposed design is based on the increase of contact surface area between target analytes and extracting phase during the sample and extracting phase transfer in microchannel. In this method, first sample solution, extracting solvent, and salt were mixed by stirrer and simultaneously delivered into a microchannel using a syringe pump. In order to optimize the influential parameters on the extraction efficiency of the proposed method, zidovudine and tenofovir disoproxil fumarate were selected as model analytes. The main parameters such as extracting solvent and its volume, salt amount, pH of sample solution, and microchannel shape, length, and its inner diameter were investigated and optimized. Under the optimized conditions, the proposed method was linear in the range of 0.1-30 µg/mL and R2 coefficients were equal to 0.9922 and 0.9947 for zidovudine and tenofovir disoproxil fumarate, respectively. Extraction efficiency of the proposed method was compared with conventional salt-assisted liquid-liquid extraction. The results show that the proposed design has higher extraction efficiency than conventional salt-assisted liquid-liquid extraction. Finally, the proposed method was successfully applied for the determination of zidovudine and tenofovir disoproxil fumarate in plasma samples.
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We developed an approach for the use of polyester dendrimer during the imprinting process to raise the number of recognized sites in the polymer matrix and improve its identification ability. Photoresponsive molecularly imprinted polymers were synthesized on modified magnetic nanoparticles involving polyester dendrimer which uses the reactivity between allyl glycidyl ether and acrylic acid for the high-yielding assembly by surface polymerization. The photoresponsive molecularly imprinted polymers were constructed using methylprednisoloneacetate as the template, water-soluble azobenzene involving 5-[(4, 3-(methacryloyloxy) phenyl) diazenyl] dihydroxy aniline as the novel functional monomer, and ethylene glycol dimethacrylate as the cross-linker. Through the evaluation of a series of features of spectroscopic and nano-structural, this sorbent showed excellent selective adsorption, recognition for the template, and provided a highly selective and sensitive strategy for determining the methylprednisoloneacetate in real and pharmaceutical samples. In addition, this sorbent according to good photo-responsive features and specific affinity to methylprednisoloneacetate with high recognition ability, represented higher binding capacity, a more extensive specific area, and faster mass transfer rate than its corresponding surface molecularly imprinted polymer.
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Dendrímeros/química , Nanopartículas de Magnetita/química , Acetato de Metilprednisolona/isolamento & purificação , Impressão Molecular , Polímeros/química , Acetato de Metilprednisolona/química , Tamanho da Partícula , Processos Fotoquímicos , Propriedades de SuperfícieRESUMO
Few-layer graphene was synthesized by in situ catalytic carbon vapor deposition (CCVD) method, using reed as a carbon source and Ni, Cu, and Mg salts as the catalyst compounds. The synthesized graphene was also used for adsorption of VOCs. Furthermore, the effect of organic additives, sorbitol, and citric acid on catalyst compounds was investigated by temperature-programmed reduction analysis (H2-TPR). The products' properties were characterized by thermo-gravimetric analysis (TGA), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and Brunauer-Emmett-Teller (BET) surface area analysis. TEM and FE-SEM images confirmed the formation of graphene sheets. Activation of the graphene by phosphoric acid at 500 °C and then by CO2 at 800 °C increased the surface area from 298 to 568 m2/g. Gasoline working capacity of the activated graphene was 65.24 g/ladsorbent. Graphical abstract Few-layer graphene was synthesized by in situ catalytic carbon vapor deposition (CCVD) method using reed as a carbon source and Ni, Cu, and Mg salts as the catalyst compounds and used for adsorption of VOCs.
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Carbono/química , Grafite/química , Poaceae/química , Compostos Orgânicos Voláteis/isolamento & purificação , Adsorção , Catálise , Ácido Cítrico/química , Cobre/química , Gases/análise , Gasolina , Magnésio/química , Microscopia Eletrônica de Varredura , Microscopia Eletrônica de Transmissão , Nanoestruturas/química , Níquel/química , Pirólise , Sorbitol/química , TermogravimetriaRESUMO
This study introduced a developed approach for dendritic ß-cyclodextrin (ß-CD) in order to obtain high sorption capacity. Synthetic strategy exploits the reactivity between acrylic acid and allyl glycidyl ether for high-yielding assembly via grafting on to the magnetic nanoparticles that are modified using 3-mercaptopropyltrimethoxysilane for various building branches and host-guest molecules of ß-CD. The methodology has been applied for the preparation of a series of ß-CD conjugated magnetic nanoparticles with dendrimers as a nano-sorbent for the extraction of methylprednisolone acetate. This study allowed us to probe (i) the effects of the dendric-cyclodextrin architecture on the affinity of sorption capacity, (ii) the drug influence between the cyclodextrin core and the polyester dendrimer, and (iii) the result of sorbent formation for using the anti-inflammatory drug as a target guest into the ring of ß-CD on biological extraction. It was found that the adsorption behavior could be fitted by the Langmuir adsorption isotherm model. The adsorption capacity of MPA is found to be 12.4 mg g-1 and indicated the homogeneous sites onto polymer grafted magnetite nano-sorbent surface. Our results confirm the high capability of this type of dendrimer-ß-CD for drug extraction in biological fluids and pharmaceutical samples. This nano-sorbent assists the magnetic solid phase extraction technique represented in the high extraction yield (up to 97%) for methylprednisolone acetate in biological human fluids and pharmaceutical samples. Moreover, the achieved polymeric nano-sorbent of the reaction combination was facilitated by a magnetic field and reusability was performed without any notable loss in the sorbent activity.
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Técnicas de Química Analítica/métodos , Dendrímeros/química , Nanopartículas de Magnetita/química , Metilprednisolona/análogos & derivados , beta-Ciclodextrinas/química , Adsorção , Óxido Ferroso-Férrico/química , Humanos , Metilprednisolona/isolamento & purificação , Acetato de Metilprednisolona , Compostos de Organossilício , Polímeros/química , Silanos , Extração em Fase SólidaRESUMO
The primary aromatic amines (PAAs) are food contaminants which may exist in packaged food. Polyurethane (PU) adhesives which are used in flexible packaging are the main source of PAAs. It is the unreacted diisocyanates which in fact migrate to foodstuff and then hydrolyze to PAAs. These PAAs include toluenediamines (TDAs) and methylenedianilines (MDAs), and the selected PAAs were 2,4-TDA, 2,6-TDA, 4,4'-MDA, 2,4'-MDA, and 2,2'-MDA. PAAs have genotoxic, carcinogenic, and allergenic effects. In this study, extraction methods were applied on a 3% acetic acid as food simulant which was spiked with the PAAs under study. Extraction methods were liquid-liquid extraction (LLE), dispersive liquid-liquid microextraction (DLLME), and solid-phase extraction (SPE) with C18 ec (octadecyl), HR-P (styrene/divinylbenzene), and SCX (strong cationic exchange) cartridges. Extracted samples were detected and analyzed by HPLC-UV. In comparison between methods, recovery rate of SCX cartridge showed the best adsorption, up to 91% for polar PAAs (TDAs and MDAs). The interested PAAs are polar and relatively soluble in water, so a cartridge with cationic exchange properties has the best absorption and consequently the best recoveries.
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This research aims at elaborating on the construction of a novel nanostructured copper oxide (Nano-CuO) sputtered thin film on the conductive fluorinated-tin oxide (FTO) layer that was exploited to immobilize glucose oxidase (GOx) enzyme via chitosan for developing impedimetric glucose biosensing. The distinct Nano-CuO thin film was fabricated by reactive DC magnetron sputtering system at the optimized instrumental deposition conditions. The FTO/Nano-CuO/Chitosan/GOx biosensor containing several layers afforded excellent microenvironment for rapid biocatalytic reaction to glucose. Field emission-scanning electron microscopy (FE-SEM), Ultraviolet-Visible spectroscopy (UV-Vis), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS) were established the morphology of modified electrode's surface and electrochemical behavior of glucose on the fabricated biosensor. Characterization of the surface morphology and roughness of CuO thin film by FE-SEM exhibits cavities of the nanoporous film as an effective biosensing area for covalent enzyme immobilization. Invented FTO/Nano-CuO/Chitosan/GOx biosensor was employed for glucose determination using the impedimetric technique. The impedimetric outcomes display high sensitivity for glucose (0.261â¯kΩâ¯perâ¯mM) detection within 0.2-15â¯mM and limit of detection as 27⯵M. The declared biosensor has been applied as a careful, noncomplicated, and exact biosensor for recognition of glucose in the real samples analysis.
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Técnicas Biossensoriais/métodos , Quitosana/química , Cobre/química , Glucose Oxidase/química , Glucose/análise , Halogenação , Compostos de Estanho/química , Técnicas Biossensoriais/instrumentação , Glicemia/análise , Eletroquímica , Eletrodos , Enzimas Imobilizadas/química , Enzimas Imobilizadas/metabolismo , Glucose Oxidase/metabolismo , Humanos , Modelos Moleculares , Nanocompostos/química , Conformação ProteicaRESUMO
The objective of this study was to identify the bioactive compounds of essential oil and evaluate the antibacterial activity of the essential oil extracted from Chenopodium album subsp. striatum against multidrug-resistant bacterial strains (MDR) which were isolated from clinical specimens by conventional methods. Furthermore, eight different Gram-negative and Gram-positive multidrug-resistant bacterial strains were used to investigate the antibacterial potential of the essential oil. The antibacterial activity was tested using MIC and MBC microdilution method, well and disc diffusion in different concentration. The hydro-distillation of aerial parts powder yield was 0.466% (v/w). Essential oil showed bactericidal activity against both MDR Gram-negative and Gram-positive bacterial strains. MIC and MBC results were ranged from 0.31 to 2.5 and 0.62 to 5.0 mg/mL. The inhibition zones in well-diffusion method were ranged from 7 ± 0.6 mm to 15 ± 1.0 mm. Disc diffusion method was ranged from 7 ± 0.0 mm to 16 ± 0.6 mm depending on the type of bacteria strain and essential oil concentration. Essential oil of Ch. album had the greatest potential to be considered as an antibacterial agent against MDR bacteria strain. This potential was due to different biological and bioactive compounds like phytol, linalool, α-terpineol and linolenic acid in the plant.
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Chenopodium album , Farmacorresistência Bacteriana Múltipla , Bactérias Gram-Negativas/efeitos dos fármacos , Bactérias Gram-Positivas/efeitos dos fármacos , Óleos Voláteis/farmacologia , Extratos Vegetais/farmacologia , Monoterpenos Acíclicos , Monoterpenos Cicloexânicos , Cicloexenos , Cromatografia Gasosa-Espectrometria de Massas , Humanos , Técnicas In Vitro , Testes de Sensibilidade Microbiana , Monoterpenos , Óleos Voláteis/análise , Óleos Voláteis/química , Fitol , Ácido alfa-LinolênicoRESUMO
A high-performance metal oxide polymer magnetite/polyethylene glycol nanocomposite was prepared and coated in situ on the surface of the optical fiber by sol-gel technology. The magnetite nanoparticles as nanofillers were synthesized by a coprecipitation method and bonded with polyethylene glycol as a polymer. The chemically bonded coating was evaluated for the headspace solid-phase microextraction of some environmentally important volatile organic compounds from aqueous samples in combination with gas chromatography and mass spectrometry. The prepared fiber was characterized by scanning electron microscopy and Fourier transform infrared spectroscopy. The mass ratio of nanofiller and polymer on the coating extraction efficiency, morphology, and stability were investigated. The parameters affecting the extraction efficiency, including the extraction time and temperature, the ionic strength, desorption temperature, and time were optimized. The sol-gelized fiber showed excellent chemical stability and longer lifespan. It also exhibited high extraction efficiency compared to the two types of commercial fibers. For volatile organic compounds analysis, the new fiber showed low detection limits (0.008-0.063 ng/L) and wide linearity (0.001-450 × 104 ng/L) under the optimized conditions. The repeatability (interday and intraday) and reproducibility were 4.13-10.08 and 5.98-11.61%, and 7.35-14.79%, respectively (n = 5). For real sample analysis, three types of water samples (ground, surface, and tap water) were studied.
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Monitoramento Ambiental/métodos , Nanocompostos/química , Polietilenoglicóis/química , Compostos Orgânicos Voláteis/análise , Poluentes Químicos da Água/análise , Água/química , Compostos Férricos/química , Óxido Ferroso-Férrico/química , Cromatografia Gasosa-Espectrometria de Massas , Reprodutibilidade dos Testes , Microextração em Fase SólidaRESUMO
A solid-phase nanoextraction method has been developed for the extraction and preconcentration of polychlorinated biphenyls using carboxyl multiwalled carbon nanotubes as a solid nano-sorbent. Parameters affecting extraction efficiency such as sorbent amount, desorption solvent type and volume, extraction time, pH, and salt content have been studied. Under optimized conditions, the correlation coefficient was up to 0.9989, the limits of detection was in the range of 1.4-3.5 ng/L, and limits of quantification was between 4.8 and 11.6 ng/L. The recoveries were in the range of 99-106% for different spiked analytes. The relative standard deviation for water samples spiked with two different spiking levels has been between 4 and 10%. The proposed sustainable method is rapid, easy to use, and small consumption of organic solvent for the detection and determination of trace levels of polychlorinated biphenyls in environmental waters.
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Free radicals play an important role in pathological processes such as aging and developing cancer; hence, natural products inhibit free radical production, and can play an important role in preventing diseases. We aimed to evaluate the scavenging activity of free radicals, reducing power, inhibition of lipid peroxidation and malondialdehyde (MDA) formation, and the antioxidant composition of rolB-transformed hairy roots and leaf callus of Catharanthus roseus. Hairy roots of the Catharanthus roseus were induced using Agrobacterium rhizogenes strain ATCC 15834 to transfer the rolB gene. Polymerase chain reaction analysis was used to identify the presence of the gene in the transformed hairy roots. Folin-Ciocalteu reagent, aluminum chloride calorimetry and high performance liquid chromatography were used to determine the content of total phenolic, flavonoid and gallic acid, respectively. To this end, we assayed the free radicals scavenging activity by 1-diphenyl-2-picrylhydrazyl (DPPH), reducing power, inhibition of lipid peroxidation and inhibition of malondialdehyde production. The results showed that phenolic, flavonoid, and gallic acid contents in the ethanol extract of the hairy roots were signiï¬cantly higher (p ≤ 0.01) than those naturally found in the extracts of root, leaf, and leaf callus of C. roseus. The hairy roots extract showed the lowest IC50 for the inhibition of DPPH(â¢). Furthermore, the ethanol extract showed the best reducing power and had the highest potential to inhibit lipid peroxidation and to form the MDA. The transformed hairy roots can be considered a rich natural source of antioxidants.
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The aim of this work was to fabricate a novel nano-fiber modified electrode, involving Lake Red C (LRC) pigments doped into electrospun polyacrylonitrile (PAN) fibrous films. Cyclic voltammetry (CV), scanning electron microscopy (SEM), electrochemical impedance spectroscopy (EIS) and differential pulse voltammetry (DPV) techniques were used for electrochemical and morphological characterization of the composite fibers. This sensor responds to Aflatoxin B1 (AFB1) over the concentration range of 40-120 nM with high accuracy and precision in analysis. The modified electrode exhibited an excellent electrocatalytic ability (α = 0.42, log K(s) = 4.21 s(-1), and Γ = 1.49 × 10(-5) mmol cm(-2)) for reduction of AFB1 at the optimum pH of 6 and working potential of -0.75 V (vs. SCE). The common substances accompanying AFB1 had no serious interferences on the response of the modified electrode to AFB1. The modified electrode indicated reproducible behavior and a high level stability during the experiments, making it particularly suitable for the analytical determination of AFB1 in poultry feed and serum samples.