Search results for: PAMAM magnetic nanoparticles
Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 2553

Search results for: PAMAM magnetic nanoparticles

2463 Paper-Based Colorimetric Sensor Utilizing Peroxidase-Mimicking Magnetic Nanoparticles Conjugated with Aptamers

Authors: Min-Ah Woo, Min-Cheol Lim, Hyun-Joo Chang, Sung-Wook Choi

Abstract:

We developed a paper-based colorimetric sensor utilizing magnetic nanoparticles conjugated with aptamers (MNP-Apts) against E. coli O157:H7. The MNP-Apts were applied to a test sample solution containing the target cells, and the solution was simply dropped onto PVDF (polyvinylidene difluoride) membrane. The membrane moves the sample radially to form the sample spots of different compounds as concentric rings, thus the MNP-Apts on the membrane enabled specific recognition of the target cells through a color ring generation by MNP-promoted colorimetric reaction of TMB (3,3',5,5'-tetramethylbenzidine) and H2O2. This method could be applied to rapidly and visually detect various bacterial pathogens in less than 1 h without cell culturing.

Keywords: aptamer, colorimetric sensor, E. coli O157:H7, magnetic nanoparticle, polyvinylidene difluoride

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2462 Monitoring Surface Modification of Polylactide Nonwoven Fabric with Weak Polyelectrolytes

Authors: Sima Shakoorjavan, Dawid Stawski, Somaye Akbari

Abstract:

In this study, great attempts have been made to initially modify polylactide (PLA) nonwoven surface with poly(amidoamine) (PAMMA) dendritic polymer to create amine active sites on PLA surface through aminolysis reaction. Further, layer-by-layer deposition of four layers of two weak polyelectrolytes, including PAMAM as polycation and polyacrylic acid (PAA) as polyanion on activated PLA, was monitored with turbidity analysis of waste-polyelectrolytes after each deposition step. The FTIR-ATR analysis confirmed the successful introduction of amine groups into PLA polymeric chains through the emerging peak around 1650 cm⁻¹ corresponding to N-H bending vibration and a double wide peak at around 3670-3170 cm⁻¹ corresponding to N-H stretching vibration. The adsorption-desorption behavior of (PAMAM) and poly (PAA) deposition was monitored by turbidity test. Turbidity results showed the desorption and removal of the previously deposited layer (second and third layers) upon the desorption of the next layers (third and fourth layers). Also, the importance of proper rinsing after aminolysis of PLA nonwoven fabric was revealed by turbidity test. Regarding the sample with insufficient rinsing process, higher desorption and removal of ungrafted PAMAM from aminolyzed-PLA surface into PAA solution was detected upon the deposition of the first PAA layer. This phenomenon can be due to electrostatic attraction between polycation (PAMAM) and polyanion (PAA). Moreover, the successful layer deposition through LBL was confirmed by the staining test of acid red 1 through spectrophotometry analysis. According to the results, layered PLA with four layers with PAMAM as the top layer showed higher dye absorption (46.7%) than neat (1.2%) and aminolyzed PLA (21.7%). In conclusion, the complicated adsorption-desorption behavior of dendritic polycation and linear polyanion systems was observed. Although desorption and removal of previously adsorbed layers occurred upon the deposition of the next layer, the remaining polyelectrolyte on the substrate is sufficient for the adsorption of the next polyelectrolyte through electrostatic attraction between oppositely charged polyelectrolytes. Also, an increase in dye adsorption confirmed more introduction of PAMAM onto PLA surface through LBL.

Keywords: surface modification, layer-by-layer technique, weak polyelectrolytes, adsorption-desorption behavior

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2461 Computer Simulation to Investigate Magnetic and Wave-Absorbing Properties of Iron Nanoparticles

Authors: Chuan-Wen Liu, Min-Hsien Liu, Chung-Chieh Tai, Bing-Cheng Kuo, Cheng-Lung Chen, Huazhen Shen

Abstract:

A recent surge in research on magnetic radar absorbing materials (RAMs) has presented researchers with new opportunities and challenges. This study was performed to gain a better understanding of the wave-absorbing phenomenon of magnetic RAMs. First, we hypothesized that the absorbing phenomenon is dependent on the particle shape. Using the Material Studio program and the micro-dot magnetic dipoles (MDMD) method, we obtained results from magnetic RAMs to support this hypothesis. The total MDMD energy of disk-like iron particles was greater than that of spherical iron particles. In addition, the particulate aggregation phenomenon decreases the wave-absorbance, according to both experiments and computational data. To conclude, this study may be of importance in terms of explaining the wave- absorbing characteristic of magnetic RAMs. Combining molecular dynamics simulation results and the theory of magnetization of magnetic dots, we investigated the magnetic properties of iron materials with different particle shapes and degrees of aggregation under external magnetic fields. The MDMD of the materials under magnetic fields of various strengths were simulated. Our results suggested that disk-like iron particles had a better magnetization than spherical iron particles. This result could be correlated with the magnetic wave- absorbing property of iron material.

Keywords: wave-absorbing property, magnetic material, micro-dot magnetic dipole, particulate aggregation

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2460 Investigation the Photocatalytic Properties of Fe3O4-ZnO Nanocomposites Prepared by Sonochemical Method

Authors: Atena Naeimi, Mehri-Sadat Ekrami-Kakhki

Abstract:

Fe3O4 is one of the important magnetic oxides with spinel structure; it has exhibited unique electric and magnetic properties based on the electron transfer between Fe2+ and Fe3+ in the octahedral sites. Fe3O4 have received considerable attention in various areas such as cancer therapy, drug targeting, enzyme immobilization catalysis, magnetic cell separation, magnetic refrigeration systems and super-paramagnetic materials. Fe3O4–ZnO nanostructures were synthesized via a surfactant-free ultrasonic reaction at room temperatures. The effect of various parameters such as temperature, time, and power on the size and morphology of the product was investigated. Alternating gradient force magnetometer shows that Fe3O4 nanoparticles exhibit super-paramagnetic behaviour at room temperature. For preparation of nanocomposite 1 g of Fe3O4 nanostructures were dispersed in 100 mL of distilled water. 0.25 g of Zn (NO3)2 and 20 mL of NH3 solution 1 M were then slowly added to the solution under ultrasonic irradiation. The product was centrifuged, washed with distilled water and dried in the air. The photocatalytic behaviour of Fe3O4–ZnO nanoparticles was evaluated using the degradation of a methyl orange aqueous solution under ultraviolet light irradiation. As time increased, more and more methyl orange was adsorbed on the nanoparticles catalyst, until the absorption peak vanish. The methyl orange concentration decreased rapidly with increasing UV-irradiation time.

Keywords: nanocomposite, ultrasonic, paramagnetic, photocatalytic

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2459 Investigation on Morphologies, Forming Mechanism, Photocatalytic and Electronic Properties of Co-Zn Ferrite Nanostructure Grown on the Reduced Graphene Oxide Support

Authors: Qinglei Liu, Ali Charkhesht, Tiva Sharifi, Ashkan Bahadoran

Abstract:

Graphene sheets are promising nanoscale building blocks as a support material for the dispersion of nanoparticles. In this work, a solvothermal method employed to directly grow Co1-xZnxFe2O4 ferrite nanospheres on graphene oxide support that is subsequently reduced to graphene. The samples morphology, structure and crystallography were investigated using field-emission scanning electron microscopy (FE-SEM) and powder X-ray diffraction (XRD). The influences of the Zn2+ content on photocatalytic activity, electrical conductivity and magnetic property of the samples are also investigated. The results showed that Co1-x Znx Fe2 O4 nanoparticles are dispersed on graphene sheets and obtained nanocomposites are soft magnetic materials. In addition the samples showed excellent photocatalytic activity under visible light irradiation.

Keywords: reduced graphene oxide, ferrite, magnetic nanocomposite, photocatalytic activity, solvothermal method

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2458 Preparation and Characterization of Dendrimer-Encapsulated Ytterbium Nanoparticles to Produce a New Nano-Radio Pharmaceutical

Authors: Aghaei Amirkhizi Navideh, Sadjadi Soodeh Sadat, Moghaddam Banaem Leila, Athari Allaf Mitra, Johari Daha Fariba

Abstract:

Dendrimers are good candidates for preparing metal nanoparticles because they can structurally and chemically well-defined templates and robust stabilizers. Poly amidoamine (PAMAM) dendrimer-based multifunctional cancer therapeutic conjugates have been designed and synthesized in pharmaceutical industry. In addition, encapsulated nanoparticle surfaces are accessible to substrates so that catalytic reactions can be carried out. For preparation of dendimer-metal nanocomposite, a dendrimer solution containing an average of 55 Yb+3 ions per dendrimer was prepared. Prior to reduction, the pH of this solution was adjusted to 7.5 using NaOH. NaBH4 was used to reduce the dendrimer-encapsulated Yb+3 to the zerovalent metal. The pH of the resulting solution was then adjusted to 3, using HClO4, to decompose excess BH4-. The UV-Vis absorption spectra of the mixture were recorded to ensure the formation of Yb-G5-NH2 complex. High-resolution electron microscopy (HRTEM) and size distribution results provide additional information about dendimer-metal nanocomposite shape, size, and size distribution of the particles. The resulting mixture was irradiated in Tehran Research Reactor 2h and neutron fluxes were 3×1011 n/cm2.Sec and the specific activity was 7MBq. Radiochemical and chemical and radionuclide quality control testes were carried. Gamma Spectroscopy and High-performance Liquid Chromatography HPLC, Thin-Layer Chromatography TLC were recorded. The injection of resulting solution to solid tumor in mice shows that it could be resized the tumor. The studies about solid tumors and nano composites show that ytterbium encapsulated-dendrimer radiopharmaceutical could be introduced as a new therapeutic for the treatment of solid tumors.

Keywords: nano-radio pharmaceutical, ytterbium, PAMAM, dendrimers

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2457 Investigation the Photocatalytic Properties of Fe3O4-TiO2 Nanocomposites Prepared by Sonochemical Method

Authors: Zh. Saffari, A. Naeimi, M. S. Ekrami-Kakhki, F. Hamidi

Abstract:

Fe3O4 is one of the important magnetic oxides with spinel structure; it has exhibited unique electric and magnetic properties based on the electron transfer between Fe2+ and Fe3+ in the octahedral sites. Fe3O4 has received considerable attention in various areas such as cancer therapy, drug targeting, enzyme immobilization catalysis, magnetic cell separation, magnetic refrigeration systems and super-paramagnetic materials Fe3O4–TiO2 nanostructures were synthesized by simple, effective and new co-precipitation method assisted by ultrasonic reaction at room temperatures with organic surfactant. The effect of various parameters such as temperature, time, and power on the size and morphology of the product was investigated. Alternating gradient force magnetometer shows that Fe3O4 nanoparticles exhibit super-paramagnetic behaviour at room temperature. For preparation of nanocomposite, 1 g of TiO2 nanostructures were dispersed in 100 mL of ethanol. 0.25 g of Fe(NO3)2 and 2 mL of octanoic acid was added to the solution as a surfactant. Then, NaOH solution (1.5 M) was slowly added into the solution until the pH of the mixture was 7–8. After complete precipitation, the solution placed under the ultrasonic irradiation for 30 min. The product was centrifuged, washed with distilled water and dried in an oven at 100 °C for 3 h. The resulting red powder was calcinated at 800 °C for 3 h to remove any organic residue. The photocatalytic behaviour of Fe3O4–TiO2 nanoparticles was evaluated using the degradation of a Methyl Violet (MV) aqueous solution under ultraviolet light irradiation. As time increased, more and more MV was adsorbed on the nanoparticles catalyst, until the absorption peak vanish. The MV concentration decreased rapidly with increasing UV-irradiation time

Keywords: magnetic, methyl violet, nanocomposite, photocatalytic

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2456 Magnetic Nano-Composite of Self-Doped Polyaniline Nanofibers for Magnetic Dispersive Micro Solid Phase Extraction Applications

Authors: Hatem I. Mokhtar, Randa A. Abd-El-Salam, Ghada M. Hadad

Abstract:

An improved nano-composite of self-doped polyaniline nanofibers and silica-coated magnetite nanoparticles were prepared and evaluated for suitability to magnetic dispersive micro solid-phase extraction. The work focused on optimization of the composite capacity to extract four fluoroquinolones (FQs) antibiotics, ciprofloxacin, enrofloxacin, danofloxacin, and difloxacin from water and improvement of composite stability towards acid and atmospheric degradation. Self-doped polyaniline nanofibers were prepared by oxidative co-polymerization of aniline with anthranilic acid. Magnetite nanopariticles were prepared by alkaline co-precipitation and coated with silica by silicate hydrolysis on magnetite nanoparticles surface at pH 6.5. The composite was formed by self-assembly by mixing self-doped polyaniline nanofibers with silica-coated magnetite nanoparticles dispersions in ethanol. The composite structure was confirmed by transmission electron microscopy (TEM). Self-doped polyaniline nanofibers and magnetite chemical structures were confirmed by FT-IR while silica coating of the magnetite was confirmed by Energy Dispersion X-ray Spectroscopy (EDS). Improved stability of the composite magnetic component was evidenced by resistance to degrade in 2N HCl solution. The adsorption capacity of self-doped polyaniline nanofibers based composite was higher than previously reported corresponding composite prepared from polyaniline nanofibers instead of self-doped polyaniline nanofibers. Adsorption-pH profile for the studied FQs on the prepared composite revealed that the best pH for adsorption was in range of 6.5 to 7. Best extraction recovery values were obtained at pH 7 using phosphate buffer. The best solvent for FQs desorption was found to be 0.1N HCl in methanol:water (8:2; v/v) mixture. 20 mL of Spiked water sample with studied FQs were preconcentrated using 4.8 mg of composite and resulting extracts were analysed by HPLC-UV method. The prepared composite represented a suitable adsorbent phase for magnetic dispersive micro-solid phase application.

Keywords: fluoroquinolones, magnetic dispersive micro extraction, nano-composite, self-doped polyaniline nanofibers

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2455 An Automated Magnetic Dispersive Solid-Phase Extraction Method for Detection of Cocaine in Human Urine

Authors: Feiyu Yang, Chunfang Ni, Rong Wang, Yun Zou, Wenbin Liu, Chenggong Zhang, Fenjin Sun, Chun Wang

Abstract:

Cocaine is the most frequently used illegal drug globally, with the global annual prevalence of cocaine used ranging from 0.3% to 0.4 % of the adult population aged 15–64 years. Growing consumption trend of abused cocaine and drug crimes are a great concern, therefore urine sample testing has become an important noninvasive sampling whereas cocaine and its metabolites (COCs) are usually present in high concentrations and relatively long detection windows. However, direct analysis of urine samples is not feasible because urine complex medium often causes low sensitivity and selectivity of the determination. On the other hand, presence of low doses of analytes in urine makes an extraction and pretreatment step important before determination. Especially, in gathered taking drug cases, the pretreatment step becomes more tedious and time-consuming. So developing a sensitive, rapid and high-throughput method for detection of COCs in human body is indispensable for law enforcement officers, treatment specialists and health officials. In this work, a new automated magnetic dispersive solid-phase extraction (MDSPE) sampling method followed by high performance liquid chromatography-mass spectrometry (HPLC-MS) was developed for quantitative enrichment of COCs from human urine, using prepared magnetic nanoparticles as absorbants. The nanoparticles were prepared by silanizing magnetic Fe3O4 nanoparticles and modifying them with divinyl benzene and vinyl pyrrolidone, which possesses the ability for specific adsorption of COCs. And this kind of magnetic particle facilitated the pretreatment steps by electromagnetically controlled extraction to achieve full automation. The proposed device significantly improved the sampling preparation efficiency with 32 samples in one batch within 40mins. Optimization of the preparation procedure for the magnetic nanoparticles was explored and the performances of magnetic nanoparticles were characterized by scanning electron microscopy, vibrating sample magnetometer and infrared spectra measurements. Several analytical experimental parameters were studied, including amount of particles, adsorption time, elution solvent, extraction and desorption kinetics, and the verification of the proposed method was accomplished. The limits of detection for the cocaine and cocaine metabolites were 0.09-1.1 ng·mL-1 with recoveries ranging from 75.1 to 105.7%. Compared to traditional sampling method, this method is time-saving and environmentally friendly. It was confirmed that the proposed automated method was a kind of highly effective way for the trace cocaine and cocaine metabolites analyses in human urine.

Keywords: automatic magnetic dispersive solid-phase extraction, cocaine detection, magnetic nanoparticles, urine sample testing

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2454 Preparation of Magnetothermally Responsive Polymer Multilayer Films for Controlled Release Applications from Surfaces

Authors: Eda Cagli, Irem Erel Goktepe

Abstract:

Externally triggered and effective release of therapeutics from polymer nanoplatforms is one of the key issues in cancer treatment. In this study, we aim to prepare polymer multilayer films which are stable at physiological conditions (little or no drug release) but release drug molecules at acidic pH and via application of AC magnetic field. First, novel stimuli responsive diblock copolymers composed of pH- and temperature-responsive blocks were synthesized. Then, block copolymer micelles with pH-responsive core and temperature responsive coronae will be obtained via pH-induced self-assembly of these block copolymers in aqueous environment. A model anticancer drug, e.g. Doxorubicin will be loaded in the micellar cores. Second, superparamagnetic nanoparticles will be synthesized. Magnetic nanoparticles and drug loaded block copolymer micelles will be used as building blocks to construct the multilayers. To mimic the acidic nature of the tumor tissues, Doxorubicin release from the micellar cores will be induced at acidic conditions. Moreover, Doxorubicin release from the multilayers will be facilitated via magnetothermal trigger. Application of AC magnetic field will induce the heating of magnetic nanoparticles resulting in an increase in the temperature of the polymer platform. This increase in temperature is expected to trigger conformational changes on the temperature-responsive micelle coronae and facilitate the release of Doxorubicin from the surface. Such polymer platform may find use in biomedical applications.

Keywords: layer-by-layer films, magnetothermal trigger, smart polymers, stimuli responsive

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2453 Magnetic Chloromethylated Polymer Nanocomposite for Selective Pollutant Removal

Authors: Fabio T. Costa, Sergio E. Moya, Marcelo H. Sousa

Abstract:

Nanocomposites designed by embedding magnetic nanoparticles into a polymeric matrix stand out as ideal magnetic-hybrid and magneto-responsive materials as sorbents for removal of pollutants in environmental applications. Covalent coupling is often desired for the immobilization of species on these nanocomposites, in order to keep them permanently bounded, not desorbing or leaching over time. Moreover, unwanted adsorbates can be separated by successive washes/magnetic separations, and it is also possible to recover the adsorbate covalently bound to the nanocomposite surface through detaching/cleavage protocols. Thus, in this work, we describe the preparation and characterization of highly-magnetizable chloromethylated polystyrene-based nanocomposite beads for selective covalent coupling in environmental applications. For synthesis optimization, acid resistant core-shelled maghemite (γ-Fe₂O₃) nanoparticles were coated with oleate molecules and directly incorporated into the organic medium during a suspension polymerization process. Moreover, the cross-linking agent ethylene glycol dimethacrylate (EGDMA) was utilized for co-polymerization with the 4-vinyl benzyl chloride (VBC) to increase the resistance of microbeads against leaching. After characterizing samples with XRD, ICP-OES, TGA, optical, SEM and TEM microscopes, a magnetic composite consisting of ~500 nm-sized cross-linked polymeric microspheres embedding ~8 nm γ-Fe₂O₃ nanoparticles was verified. This nanocomposite showed large room temperature magnetization (~24 emu/g) due to the high content in maghemite (~45 wt%) and resistance against leaching even in acidic media. Moreover, the presence of superficial chloromethyl groups, probed by FTIR and XPS spectroscopies and confirmed by an amination test can selectively adsorb molecules through the covalent coupling and be used in molecular separations as shown for the selective removal of 4-aminobenzoic acid from a mixture with benzoic acid.

Keywords: nanocomposite, magnetic nanoparticle, covalent separation, pollutant removal

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2452 Application of Functionalized Magnetic Particles as Demulsifier for Oil‐in‐Water Emulsions

Authors: Hamideh Hamedi, Nima Rezaei, Sohrab Zendehboudi

Abstract:

Separating emulsified oil contaminations from waste- or produced water is of interest to various industries. Magnetic particles (MPs) application for separating dispersed and emulsified oil from wastewater is becoming more popular. Stabilization of MPs is required through developing a coating layer on their surfaces to prevent their agglomeration and enhance their dispersibility. In this research, we study the effects of coating material, size, and concentration of iron oxide MPs on oil separation efficiency, using oil adsorption capacity measurements. We functionalize both micro-and nanoparticles of Fe3O4 using sodium dodecyl sulfate (SDS) as an anionic surfactant, cetyltrimethylammonium bromide (CTAB) as a cationic surfactant, and stearic acid (SA). The chemical structures and morphologies of these particles are characterized using Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), and Energy Dispersive X-ray (EDX). The oil-water separation results indicate that a low dosage of the coated magnetic nanoparticle with CTAB (0.5 g/L MNP-CTAB) results the highest oil adsorption capacity (nearly 100%) for 1000 ppm dodecane-in-water emulsion, containing ultra-small droplets (250–300 nm). While separation efficiency of the same dosage of bare MNPs is around 57.5%. Demulsification results of magnetic microparticles (MMPs) also reveal that the functionalizing particles with CTAB increase oil removal efficiency from 86.3% for bare MMP to 92% for MMP-CTAB. Comparing the results of different coating materials implies that the major interaction reaction is an electrostatic attraction between negatively charged oil droplets and positively charged MNP-CTAB and MMP-CTAB. Furthermore, the synthesized nanoparticles could be recycled and reused; after ten cycles the oil adsorption capacity slightly decreases to near 95%. In conclusion, functionalized magnetic particles with high oil separation efficiency could be used effectively in treatment of oily wastewater. Finally, optimization of the adsorption process is required by considering the effective system variables, and fluid properties.

Keywords: oily wastewater treatment, emulsions, oil-water separation, adsorption, magnetic nanoparticles

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2451 Dielectric, Electrical and Magnetic Properties of Elastomer Filled with in situ Thermally Reduced Graphene Oxide and Spinel Ferrite NiFe₂O₄ Nanoparticles

Authors: Raghvendra Singh Yadav, Ivo Kuritka, Jarmila Vilcakova, Pavel Urbanek, Michal Machovsky, David Skoda, Milan Masar

Abstract:

The elastomer nanocomposites were synthesized by solution mixing method with an elastomer as a matrix and in situ thermally reduced graphene oxide (RGO) and spinel ferrite NiFe₂O₄ nanoparticles as filler. Spinel ferrite NiFe₂O₄ nanoparticles were prepared by the starch-assisted sol-gel auto-combustion method. The influence of filler on the microstructure, morphology, dielectric, electrical and magnetic properties of Reduced Graphene Oxide-Nickel Ferrite-Elastomer nanocomposite was characterized by X-ray diffraction, Raman spectroscopy, Fourier transform infrared spectroscopy, field emission scanning electron microscopy, X-ray photoelectron spectroscopy, the Dielectric Impedance analyzer, and vibrating sample magnetometer. Scanning electron microscopy study revealed that the fillers were incorporated in elastomer matrix homogeneously. The dielectric constant and dielectric tangent loss of nanocomposites was decreased with the increase of frequency, whereas, the dielectric constant increases with the addition of filler. Further, AC conductivity was increased with the increase of frequency and addition of fillers. Furthermore, the prepared nanocomposites exhibited ferromagnetic behavior. This work was supported by the Ministry of Education, Youth and Sports of the Czech Republic – Program NPU I (LO1504).

Keywords: polymer-matrix composites, nanoparticles as filler, dielectric property, magnetic property

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2450 Towards the Integration of a Micro Pump in μTAS

Authors: Y. Haik

Abstract:

The objective of this study is to present a micro mechanical pump that was fabricated using SwIFT™ microfabrication surface micromachining process and to demonstrate the feasibility of integrating such micro pump into a micro analysis system. The micropump circulates the bio-sample and magnetic nanoparticles through different compartments to separate and purify the targeted bio-sample. This article reports the flow characteristics in the microchannels and in a crescent micro pump.

Keywords: crescent micropumps, microanalysis, nanoparticles, MEMS

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2449 Speciation, Preconcentration, and Determination of Iron(II) and (III) Using 1,10-Phenanthroline Immobilized on Alumina-Coated Magnetite Nanoparticles as a Solid Phase Extraction Sorbent in Pharmaceutical Products

Authors: Hossein Tavallali, Mohammad Ali Karimi, Gohar Deilamy-Rad

Abstract:

The proposed method for speciation, preconcentration and determination of Fe(II) and Fe(III) in pharmaceutical products was developed using of alumina-coated magnetite nanoparticles (Fe3O4/Al2O3 NPs) as solid phase extraction (SPE) sorbent in magnetic mixed hemimicell solid phase extraction (MMHSPE) technique followed by flame atomic absorption spectrometry analysis. The procedure is based on complexation of Fe(II) with 1, 10-phenanthroline (OP) as complexing reagent for Fe(II) that immobilized on the modified Fe3O4/Al2O3 NPs. The extraction and concentration process for pharmaceutical sample was carried out in a single step by mixing the extraction solvent, magnetic adsorbents under ultrasonic action. Then, the adsorbents were isolated from the complicated matrix easily with an external magnetic field. Fe(III) ions determined after facility reduced to Fe(II) by added a proper reduction agent to sample solutions. Compared with traditional methods, the MMHSPE method simplified the operation procedure and reduced the analysis time. Various influencing parameters on the speciation and preconcentration of trace iron, such as pH, sample volume, amount of sorbent, type and concentration of eluent, were studied. Under the optimized operating conditions, the preconcentration factor of the modified nano magnetite for Fe(II) 167 sample was obtained. The detection limits and linear range of this method for iron were 1.0 and 9.0 - 175 ng.mL−1, respectively. Also the relative standard deviation for five replicate determinations of 30.00 ng.mL-1 Fe2+ was 2.3%.

Keywords: Alumina-Coated magnetite nanoparticles, Magnetic Mixed Hemimicell Solid-Phase Extraction, Fe(ΙΙ) and Fe(ΙΙΙ), pharmaceutical sample

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2448 Magnetic SF (Silk Fibroin) E-Gel Scaffolds Containing bFGF-Conjugated Fe3O4 Nanoparticles

Authors: Z. Karahaliloğlu, E. Yalçın, M. Demirbilek, E.B. Denkbaş

Abstract:

Critical-sized bone defects caused by trauma, bone diseases, prosthetic implant revision or tumor excision cannot be repaired by physiological regenerative processes. Current orthopedic applications for critical-sized bone defects are to use autologous bone grafts, bone allografts, or synthetic graft materials. However, these strategies are unable to solve completely the problem, and motivate the development of novel effective biological scaffolds for tissue engineering applications and regenerative medicine applications. In particular, scaffolds combined with a variety of bio-agents as fundamental tools emerge to provide the regeneration of damaged bone tissues due to their ability to promote cell growth and function. In this study, a magnetic silk fibroin (SF) hydrogel scaffold was prepared by electrogelation process of the concentrated Bombxy mori silk fibroin (8 %wt) aqueous solution. For enhancement of osteoblast-like cells (SaOS-2) growth and adhesion, basal fibroblast growth factor (bFGF) were conjugated physically to the HSA-coated magnetic nanoparticles (Fe3O4) and magnetic SF e-gel scaffolds were prepared by incorporation of Fe3O4, HSA (human serum albumin)=Fe3O4 and HSA=Fe3O4-bFGF nanoparticles. HSA=Fe3O4, HSA=Fe3O4-bFGF loaded and bare SF e-gels scaffolds were characterized using scanning electron microscopy (SEM.) For cell studies, human osteoblast-like cell line (SaOS-2) was used and an MTT assay was used to assess the cytotoxicity of magnetic silk fibroin e-gel scaffolds and cell density on these surfaces. For the evaluation osteogenic activation, ALP (alkaline phosphatase), the amount of mineralized calcium, total protein and collagen were studied. Fe3O4 nanoparticles were successfully synthesized and bFGF was conjugated to HSA=Fe3O4 nanoparticles with %97.5 of binding yield which has a particle size of 71.52±2.3 nm. Electron microscopy images of the prepared HSA and bFGF incorporated SF e-gel scaffolds showed a 3D porous morphology. In terms of water uptake results, bFGF conjugated HSA=Fe3O4 nanoparticles has the best water absorbability behavior among all groups. In the in-vitro cell culture studies realized using SaOS-2 cell line, the coating of Fe3O4 nanoparticles surface with a protein enhance the cell viability and HSA coating and bFGF conjugation, the both have an inductive effect in the cell proliferation. One of the markers of bone formation and osteoblast differentiation, according to the ALP activity and total protein results, HSA=Fe3O4-bFGF loaded SF e-gels had significantly enhanced ALP activity. Osteoblast cultured HSA=Fe3O4-bFGF loaded SF e-gels deposited more calcium compared with SF e-gel. The proposed magnetic scaffolds seem to be promising for bone tissue regeneration and used in future work for various applications.

Keywords: basic fibroblast growth factor (bFGF), e-gel, iron oxide nanoparticles, silk fibroin

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2447 The Influence of Reaction Parameters on Magnetic Properties of Synthesized Strontium Ferrite

Authors: M. Bahgat, F. M. Awan, H. A. Hanafy

Abstract:

The conventional ceramic route was utilized to prepare a hard magnetic powder (M-type strontium ferrite, SrFe12O19). The stoichiometric mixture of iron oxide and strontium carbonate were calcined at 1000°C and then fired at various temperatures. The influence of various reaction parameters such as mixing ratio, calcination temperature, firing temperature and firing time on the magnetic behaviors of the synthesized magnetic powder were investigated.The magnetic properties including Coercivity (Hc), Magnetic saturation (Ms), and Magnetic remnance (Mr) were measured by vibrating sample magnetometer. Morphologically the produced magnetic powder has a dense hexagonal grain shape structure.

Keywords: hard magnetic materials, ceramic route, strontium ferrite, magnetic properties

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2446 Functionalization of Carbon-Coated Iron Nanoparticles with Fluorescent Protein

Authors: A. G. Pershina, P. S. Postnikov, M. E. Trusova, D. O. Burlakova, A. E. Sazonov

Abstract:

Invention of magnetic-fluorescent nanocomposites is a rapidly developing area of research. The magnetic-fluorescent nanocomposite attractiveness is connected with the ability of simultaneous management and control of such nanocomposites by two independent methods based on different physical principles. These nanocomposites are applied for the solution of various essential scientific and experimental biomedical problems. The aim of this research is development of principle approach to nanobiohybrid structures with magnetic and fluorescent properties design. The surface of carbon-coated iron nanoparticles (Fe@C) were covalently modified by 4-carboxy benzenediazonium tosylate. Recombinant fluorescent protein TagGFP2 (Eurogen) was obtained in E. coli (Rosetta DE3) by standard laboratory techniques. Immobilization of TagGFP2 on the nanoparticles surface was provided by the carbodiimide activation. The amount of COOH-groups on the nanoparticle surface was estimated by elemental analysis (Elementar Vario Macro) and TGA-analysis (SDT Q600, TA Instruments. Obtained nanocomposites were analyzed by FTIR spectroscopy (Nicolet Thermo 5700) and fluorescence microscopy (AxioImager M1, Carl Zeiss). Amount of the protein immobilized on the modified nanoparticle surface was determined by fluorimetry (Cary Eclipse) and spectrophotometry (Unico 2800) with the help of preliminary obtained calibration plots. In the FTIR spectra of modified nanoparticles the adsorption band of –COOH group around 1700 cm-1 and bands in the region of 450-850 cm-1 caused by bending vibrations of benzene ring were observed. The calculated quantity of active groups on the surface was equal to 0,1 mmol/g of material. The carbodiimide activation of COOH-groups on nanoparticles surface results to covalent immobilization of TagGFP2 fluorescent protein (0.2 nmol/mg). The success of immobilization was proved by FTIR spectroscopy. Protein characteristic adsorption bands in the region of 1500-1600 cm-1 (amide I) were presented in the FTIR spectrum of nanocomposite. The fluorescence microscopy analysis shows that Fe@C-TagGFP2 nanocomposite possesses fluorescence properties. This fact confirms that TagGFP2 protein retains its conformation due to immobilization on nanoparticles surface. Magnetic-fluorescent nanocomposite was obtained as a result of unique design solution implementation – the fluorescent protein molecules were fixed to the surface of superparamagnetic carbon-coated iron nanoparticles using original diazonium salts.

Keywords: carbon-coated iron nanoparticles, diazonium salts, fluorescent protein, immobilization

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2445 Synthetic Bis(2-Pyridylmethyl)Amino-Chloroacetyl Chloride- Ethylenediamine-Grafted Graphene Oxide Sheets Combined with Magnetic Nanoparticles: Remove Metal Ions and Catalytic Application

Authors: Laroussi Chaabane, Amel El Ghali, Emmanuel Beyou, Mohamed Hassen V. Baouab

Abstract:

In this research, the functionalization of graphene oxide sheets by ethylenediamine (EDA) was accomplished and followed by the grafting of bis(2-pyridylmethyl) amino group (BPED) onto the activated graphene oxide sheets in the presence of chloroacetylchloride (CAC) and then combined with magnetic nanoparticles (Fe₃O₄NPs) to produce a magnetic graphene-based composite [(Go-EDA-CAC)@Fe₃O₄NPs-BPED]. The physicochemical properties of [(Go-EDA-CAC)@Fe₃O₄NPs-BPED] composites were investigated by Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA). Additionally, the catalysts can be easily recycled within ten seconds by using an external magnetic field. Moreover, [(Go-EDA-CAC)@Fe₃O₄NPs-BPED] was used for removing Cu(II) ions from aqueous solutions using a batch process. The effect of pH, contact time and temperature on the metal ions adsorption were investigated, however weakly dependent on ionic strength. The maximum adsorption capacity values of Cu(II) on the [(Go-EDA-CAC)@Fe₃O₄NPs-BPED] at the pH of 6 is 3.46 mmol.g⁻¹. To examine the underlying mechanism of the adsorption process, pseudo-first, pseudo-second-order, and intraparticle diffusion models were fitted to experimental kinetic data. Results showed that the pseudo-second-order equation was appropriate to describe the Cu (II) adsorption by [(Go-EDA-CAC)@Fe₃O₄NPs-BPED]. Adsorption data were further analyzed by the Langmuir, Freundlich, and Jossens adsorption approaches. Additionally, the adsorption properties of the [(Go-EDA-CAC)@Fe₃O₄NPs-BPED], their reusability (more than 6 cycles) and durability in the aqueous solutions open the path to removal of Cu(II) from water solution. Based on the results obtained, we report the activity of Cu(II) supported on [(Go-EDA-CAC)@Fe₃O₄NPs-BPED] as a catalyst for the cross-coupling of symmetric alkynes.

Keywords: graphene, magnetic nanoparticles, adsorption kinetics/isotherms, cross coupling

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2444 An Aptasensor Based on Magnetic Relaxation Switch and Controlled Magnetic Separation for the Sensitive Detection of Pseudomonas aeruginosa

Authors: Fei Jia, Xingjian Bai, Xiaowei Zhang, Wenjie Yan, Ruitong Dai, Xingmin Li, Jozef Kokini

Abstract:

Pseudomonas aeruginosa is a Gram-negative, aerobic, opportunistic human pathogen that is present in the soil, water, and food. This microbe has been recognized as a representative food-borne spoilage bacterium that can lead to many types of infections. Considering the casualties and property loss caused by P. aeruginosa, the development of a rapid and reliable technique for the detection of P. aeruginosa is crucial. The whole-cell aptasensor, an emerging biosensor using aptamer as a capture probe to bind to the whole cell, for food-borne pathogens detection has attracted much attention due to its convenience and high sensitivity. Here, a low-field magnetic resonance imaging (LF-MRI) aptasensor for the rapid detection of P. aeruginosa was developed. The basic detection principle of the magnetic relaxation switch (MRSw) nanosensor lies on the ‘T₂-shortening’ effect of magnetic nanoparticles in NMR measurements. Briefly speaking, the transverse relaxation time (T₂) of neighboring water protons get shortened when magnetic nanoparticles are clustered due to the cross-linking upon the recognition and binding of biological targets, or simply when the concentration of the magnetic nanoparticles increased. Such shortening is related to both the state change (aggregation or dissociation) and the concentration change of magnetic nanoparticles and can be detected using NMR relaxometry or MRI scanners. In this work, two different sizes of magnetic nanoparticles, which are 10 nm (MN₁₀) and 400 nm (MN₄₀₀) in diameter, were first immobilized with anti- P. aeruginosa aptamer through 1-Ethyl-3-(3-dimethylaminopropyl) carbodiimide (EDC)/N-hydroxysuccinimide (NHS) chemistry separately, to capture and enrich the P. aeruginosa cells. When incubating with the target, a ‘sandwich’ (MN₁₀-bacteria-MN₄₀₀) complex are formed driven by the bonding of MN400 with P. aeruginosa through aptamer recognition, as well as the conjugate aggregation of MN₁₀ on the surface of P. aeruginosa. Due to the different magnetic performance of the MN₁₀ and MN₄₀₀ in the magnetic field caused by their different saturation magnetization, the MN₁₀-bacteria-MN₄₀₀ complex, as well as the unreacted MN₄₀₀ in the solution, can be quickly removed by magnetic separation, and as a result, only unreacted MN₁₀ remain in the solution. The remaining MN₁₀, which are superparamagnetic and stable in low field magnetic field, work as a signal readout for T₂ measurement. Under the optimum condition, the LF-MRI platform provides both image analysis and quantitative detection of P. aeruginosa, with the detection limit as low as 100 cfu/mL. The feasibility and specificity of the aptasensor are demonstrated in detecting real food samples and validated by using plate counting methods. Only two steps and less than 2 hours needed for the detection procedure, this robust aptasensor can detect P. aeruginosa with a wide linear range from 3.1 ×10² cfu/mL to 3.1 ×10⁷ cfu/mL, which is superior to conventional plate counting method and other molecular biology testing assay. Moreover, the aptasensor has a potential to detect other bacteria or toxins by changing suitable aptamers. Considering the excellent accuracy, feasibility, and practicality, the whole-cell aptasensor provides a promising platform for a quick, direct and accurate determination of food-borne pathogens at cell-level.

Keywords: magnetic resonance imaging, meat spoilage, P. aeruginosa, transverse relaxation time

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2443 Electrical Properties of Cement-Based Piezoelectric Nanoparticles

Authors: Moustafa Shawkey, Ahmed G. El-Deen, H. M. Mahmoud, M. M. Rashad

Abstract:

Piezoelectric based cement nanocomposite is a promising technology for generating an electric charge upon mechanical stress of concrete structure. Moreover, piezoelectric nanomaterials play a vital role for providing accurate system of structural health monitoring (SHM) of the concrete structure. In light of increasing awareness of environmental protection and energy crises, generating renewable and green energy form cement based on piezoelectric nanomaterials attracts the attention of the researchers. Herein, we introduce a facial synthesis for bismuth ferrite nanoparticles (BiFeO3 NPs) as piezoelectric nanomaterial via sol gel strategy. The fabricated piezoelectric nanoparticles are uniformly distributed to cement-based nanomaterials with different ratios. The morphological shape was characterized by field emission scanning electron microscopy (FESEM) and high-resolution transmission electron microscopy (HR-TEM) as well as the crystal structure has been confirmed using X-ray diffraction (XRD). The ferroelectric and magnetic behaviours of BiFeO3 NPs have been investigated. Then, dielectric constant for the prepared cement samples nanocomposites (εr) is calculated. Intercalating BiFeO3 NPs into cement materials achieved remarkable results as piezoelectric cement materials, distinct enhancement in ferroelectric and magnetic properties. Overall, this present study introduces an effective approach to improve the electrical properties based cement applications.

Keywords: piezoelectric nanomaterials, cement technology, bismuth ferrite nanoparticles, dielectric

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2442 Magnetic Activated Carbon: Preparation, Characterization, and Application for Vanadium Removal

Authors: Hakimeh Sharififard, Mansooreh Soleimani

Abstract:

In this work, the magnetic activated carbon nanocomposite (Fe-CAC) has been synthesized by anchorage iron hydr(oxide) nanoparticles onto commercial activated carbon (CAC) surface and characterized using BET, XRF, SEM techniques. The influence of various removal parameters such as pH, contact time and initial concentration of vanadium on vanadium removal was evaluated using CAC and Fe-CAC in batch method. The sorption isotherms were studied using Langmuir, Freundlich and Dubinin–Radushkevich (D–R) isotherm models. These equilibrium data were well described by the Freundlich model. Results showed that CAC had the vanadium adsorption capacity of 37.87 mg/g, while the Fe-AC was able to adsorb 119.01 mg/g of vanadium. Kinetic data was found to confirm pseudo-second-order kinetic model for both adsorbents.

Keywords: magnetic activated carbon, remove, vanadium, nanocomposite, freundlich

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2441 Analytical Model for Vacuum Cathode Arcs in an Oblique Magnetic Field

Authors: P. W. Chen, C. T. Chang, Y. Peng, J. Y. Wu, D. J. Jan, Md. Manirul Ali

Abstract:

In the last decade, the nature of cathode spot splitting and the current per spot depended on an oblique magnetic field was investigated. This model for cathode current splitting is developed that we have investigated with relationship the magnetic pressures produced by kinetic pressure, self-magnetic pressure, and changed with an external magnetic field. We propose a theoretical model that has been established to an external magnetic field with components normal and tangential to the cathode surface influenced on magnetic pressure strength. We mainly focus on developed to understand the current per spot influenced with the tangential magnetic field strength and normal magnetic field strength.

Keywords: cathode spot, vacuum arc discharge, oblique magnetic field, tangential magnetic field

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2440 Consideration of Magnetic Lines of Force as Magnets Produced by Percussion Waves

Authors: Angel Pérez Sánchez

Abstract:

Background: Consider magnetic lines of force as a vector magnetic current was introduced by convention around 1830. But this leads to a dead end in traditional physics, and quantum explanations must be referred to explain the magnetic phenomenon. However, a study of magnetic lines as percussive waves leads to other paths capable of interpreting magnetism through traditional physics. Methodology: Brick used in the experiment: two parallel electric current cables attract each other if current goes in the same direction and its application at a microscopic level inside magnets. Significance: Consideration of magnetic lines as magnets themselves would mean a paradigm shift in the study of magnetism and open the way to provide solutions to mysteries of magnetism until now only revealed by quantum mechanics. Major findings: discover how a magnetic field is created, as well as reason how magnetic attraction and repulsion work, understand how magnets behave when splitting them, and reveal the impossibility of a Magnetic Monopole. All of this is presented as if it were a symphony in which all the notes fit together perfectly to create a beautiful, smart, and simple work.

Keywords: magnetic lines of force, magnetic field, magnetic attraction and repulsion, magnet split, magnetic monopole, magnetic lines of force as magnets, magnetic lines of force as waves

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2439 Synthesis and Characterization of Silver Nanoparticles Using Daucus carota Extract

Authors: M. R. Bindhu, M. Umadevi

Abstract:

Silver nanoparticles have been synthesized by Daucus carota extract as reducing agent was reported here. The involvement of phytochemicals in the Daucus carota extract in the reduction and stabilization of silver nanoparticles has been established using XRD and UV-vis studies. The UV-vis spectrum of the prepared silver nanoparticles showed surface plasmon absorbance peak at 450 nm. The obtained silver nanoparticles were almost spherical in shape with the average size of 15 nm. Crystalline nature of the nanoparticles was evident from bright spots in the SAED pattern and peaks in the XRD pattern. This new, simple and natural method for biosynthesis of silver nanoparticles offers a valuable contribution in the area of green synthesis and nanotechnology avoiding the presence of hazardous and toxic solvents and waste.

Keywords: Daucus carota, green synthesis, silver nanoparticles, surface plasmon resonance

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2438 Chitosan Functionalized Fe3O4@Au Core-Shell Nanomaterials for Targeted Drug Delivery

Authors: S. S. Pati, L. Herojit Singh, A. C. Oliveira, V. K. Garg

Abstract:

Chitosan functionalized Fe3O4-Au core shell nanoparticles have been prepared using a two step wet chemical approach using NaBH4 as reducing agent for formation of Au inethylene glycol. X-ray diffraction studies shows individual phases of Fe3O4 and Au in the as prepared samples with crystallite size of 5.9 and 11.4 nm respectively. The functionalization of the core-shell nanostructure with Chitosan has been confirmed using Fourier transform infrared spectroscopy along with signatures of octahedral and tetrahedral sites of Fe3O4 below 600cm-1. Mössbauer spectroscopy shows decrease in particle-particle interaction in presence of Au shell (72% sextet) than pure oleic coated Fe3O4 nanoparticles (88% sextet) at room temperature. At 80K, oleic acid coated Fe3O4 shows only sextets whereas the Chitosan functionalized Fe3O4 and Chitosan functionalized Fe3O4@Au core shell show presence of 5 and 11% doublet, respectively.

Keywords: core shell, drug delivery, gold nanoparticles, magnetic nanoparticles

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2437 Fe₃O₄/SiO₂/TiO₂ Nanoparticles as Catalyst for Recovery of Gold from the Mixture of Au(III) and Cu(II) Ions

Authors: Eko S. Kunarti, Akhmad Syoufian, Indriana Kartini, Agnes

Abstract:

Fe₃O₄/SiO₂/TiO₂ nanoparticles have been synthesized and applied as a photocatalyst for the recovery of gold from the mixture of Au(III) and Cu(II) ions. The synthesis was started by the preparation of magnetite (Fe₃O₄) using coprecipitation and sonication methods, followed by SiO₂ coating on magnetite using sol-gel reactions, and then TiO₂ coating using sol-gel process. Characterization was performed by using infrared spectroscopy, X-ray diffraction, transmission electron microscopy methods. Activity of Fe₃O₄/SiO₂/TiO₂ nanoparticles was evaluated as a photocatalyst for recovery of gold through photoreduction of Au(III) ions in Au(III) and Cu(II) ions mixture with a ratio of 1:1, in a closed reactor equipped with UV lamp. The photoreduction yield was represented as a percentage (%) of reduced Au(III) which was calculated by substraction of initial Au(III) concentration by the unreduced one. The unreduced Au(III) was determined by atomic absorption spectrometry. Results showed that the Fe₃O₄/SiO₂/TiO₂ nanoparticles were successfully synthesised with excellent magnetic and photocatalytic properties. The nanoparticles present optimum activity at a pH of 5 under UV irradiation for 120 minutes. At the optimum condition, the Fe₃O₄/SiO₂/TiO₂ nanoparticles could reduce Au³⁺ to Au⁰ 97.24%. In the mixture of Au(III) and Cu(II) ions, the Au(III) ions are more easily reducible than Cu(II) ions with the reduction results of 96.9% and 45.80% for Au(III) and Cu(II) ions, respectively. In addition, the presence of Cu(II) ions has no significant effect on the amount of gold recovered and its reduction reaction rate.

Keywords: Fe₃O₄/SiO₂/TiO₂, photocatalyst, recovery, gold, Au(III) and Cu(II) mixture

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2436 Magnetic Bio-Nano-Fluids for Hyperthermia

Authors: Z. Kolacinski, L. Szymanski. G. Raniszewski, D. Koza, L. Pietrzak

Abstract:

Magnetic Bio-Nano-Fluid (BNF) can be composed of a buffer fluid such as plasma and magnetic nanoparticles such as iron, nickel, cobalt and their oxides. However iron is one of the best elements for magnetization by electromagnetic radiation. It can be used as a tool for medical diagnosis and treatment. Radio frequency (RF) radiation is able to heat iron nanoparticles due to magnetic hysteresis. Electromagnetic heating of iron nanoparticles and ferro-fluids BNF can be successfully used for non-invasive thermal ablation of cancer cells. Moreover iron atoms can be carried by carbon nanotubes (CNTs) if iron is used as catalyst for CNTs synthesis. Then CNTs became the iron containers and they screen the iron content against oxidation. We will present a method of CNTs addressing to the required cells. For thermal ablation of cancer cells we use radio frequencies for which the interaction with human body should be limited to minimum. Generally, the application of RF energy fields for medical treatment is justified by deep tissue penetration. The highly iron doped CNTs as the carriers creating magnetic fluid will be presented. An excessive catalyst injection method using electrical furnace and microwave plasma reactor will be presented. This way it is possible to grow the Fe filled CNTs on a moving surface in continuous synthesis process. This also allows producing uniform carpet of the Fe filled CNTs carriers. For the experimental work targeted to cell ablation we used RF generator to measure the increase in temperature for some samples like: solution of Fe2O3 in BNF which can be plasma-like buffer, solutions of pure iron of different concentrations in plasma-like buffer and in buffer used for a cell culture, solutions of carbon nanotubes (MWCNTs) of different concentrations in plasma-like buffer and in buffer used for a cell culture. Then the targeted therapies which can be effective if the carriers are able to distinguish the difference between cancerous and healthy cell’s physiology are considered. We have developed an approach based on ligand-receptor or antibody-antigen interactions for the case of colon cancer.

Keywords: cancer treatment, carbon nano tubes, drag delivery, hyperthermia, iron

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2435 Adsorption and Selective Determination Ametryne in Food Sample Using of Magnetically Separable Molecular Imprinted Polymers

Authors: Sajjad Hussain, Sabir Khan, Maria Del Pilar Taboada Sotomayor

Abstract:

This work demonstrates the synthesis of magnetic molecularly imprinted polymers (MMIPs) for determination of a selected pesticide (ametryne) using high performance liquid chromatography (HPLC). Computational simulation can assist the choice of the most suitable monomer for the synthesis of polymers. The (MMIPs) were polymerized at the surface of Fe3O4@SiO2 magnetic nanoparticles (MNPs) using 2-vinylpyradine as functional monomer, ethylene-glycol-dimethacrylate (EGDMA) is a cross-linking agent and 2,2-Azobisisobutyronitrile (AIBN) used as radical initiator. Magnetic non-molecularly imprinted polymer (MNIPs) was also prepared under the same conditions without analyte. The MMIPs were characterized by scanning electron microscopy (SEM), Brunauer, Emmett and Teller (BET) and Fourier transform infrared spectroscopy (FTIR). Pseudo first order and pseudo second order model were applied to study kinetics of adsorption and it was found that adsorption process followed the pseudo first order kinetic model. Adsorption equilibrium data was fitted to Freundlich and Langmuir isotherms and the sorption equilibrium process was well described by Langmuir isotherm mode. The selectivity coefficients (α) of MMIPs for ametryne with respect to atrazine, ciprofloxacin and folic acid were 4.28, 12.32, and 14.53 respectively. The spiked recoveries ranged between 91.33 and 106.80% were obtained. The results showed high affinity and selectivity of MMIPs for pesticide ametryne in the food samples.

Keywords: molecularly imprinted polymer, pesticides, magnetic nanoparticles, adsorption

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2434 Synthesis and Catalytic Activity of N-Heterocyclic Carbene Copper Catalysts Supported on Magnetic Nanoparticles

Authors: Iwona Misztalewska-Turkowicz, Agnieszka Z. Wilczewska, Karolina H. Markiewicz

Abstract:

Carbenes - species which possess neutral carbon atom with two shared and two unshared valence electrons, are known for their high reactivity and instability. Nevertheless, it is also known, that some carbenes i.e. N-heterocyclic carbenes (NHCs), can form stable crystals. The usability of NHCs in organic synthesis was studied. Due to their exceptional properties (high nucleophilicity) NHCs are commonly used as organocatalysts and also as ligands in transition metal complexes. NHC ligands possess better electron-donating properties than phosphines. Moreover, they exhibit lower toxicity. Due to these features, phosphines are frequently replaced by NHC ligands. In this research is discussed the synthesis of five-membered NHCs which are mainly obtained by deprotonation of azolium salts, e.g., imidazolium or imidazolinium salts. Some of them are immobilized on a solid support what leads to formation of heterogeneous, recyclable catalysts. Magnetic nanoparticles (MNPs) are often used as a solid support for catalysts. MNPs can be easily separated from the reaction mixture using an external magnetic field. Due to their low size and high surface to volume ratio, they are a good choice for immobilization of catalysts. Herein is presented synthesis of N-heterocyclic carbene copper complexes directly on the surface of magnetic nanoparticles. Formation of four different catalysts is discussed. They vary in copper oxidation state (Cu(I) and Cu(II)) and structure of NHC ligand. Catalysts were tested in Huisgen reaction, a type of copper catalyzed azide-alkyne cycloaddition (CuAAC) reaction. Huisgen reaction represents one of the few universal and highly efficient reactions in which 1,2,3-triazoles can be obtained. The catalytic activity of all synthesized catalysts was compared with activity of commercially available ones. Different reaction conditions (solvent, temperature, the addition of reductant) and reusability of the obtained catalysts were investigated and are discussed. The project was financially supported by National Science Centre, Poland, grant no. 2016/21/N/ST5/01316. Analyses were performed in Centre of Synthesis and Analyses BioNanoTechno of University of Bialystok. The equipment in the Centre of Synthesis and Analysis BioNanoTechno of University of Bialystok was funded by EU, as a part of the Operational Program Development of Eastern Poland 2007-2013, project: POPW.01.03.00-20-034/09-00 and POPW.01.03.00-20-004/11.

Keywords: N-heterocyclic carbenes, click reaction, magnetic nanoparticles, copper catalysts

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