Magnetic nanoparticles (Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> &amp; Co<Subscript>3</Subscript>O<Subscript>4</Subscript>) and their applications in urea biosensing

Nanobiotechnology has opened a new and exciting opportunities for exploring urea biosensor based on magnetic nanoparticles (NPs) mainly Fe₃O₄ and Co₃O₄. These NPs have been extensively exploited to develop biosensors with stability, selectivity, reproducibility and fast response time. This review gives an overview of the development of urea biosensor based on Fe₃O₄ and Co₃O₄ for in vitro diagnostic applications along with significant improvements over the last few decades. Additionally, effort has been made to elaborate properties of magnetic nanoparticles (MNPs) in biosensing aspects. It also gives details of recent developments in hybrid nanobiocomposite based urea biosensor.     

Thiol-functionalized Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>/SiO<Subscript>2</Subscript> microspheres with superparamagnetism and their adsorption properties for Au(III) ion separation

Thiol-functionalized Fe₃O₄/SiO₂ microspheres (Fe₃O₄/SiO₂-SH) with high saturation magnetization (69.3 emu g^–1), superparamagnetism, and good dispersibility have been prepared by an ethylene glycol reduction method in combination with a modified Stöber method. The as-prepared composite magnetic spheres are characterized with fourier transform infrared spectroscopy (FT-IR), zeta potential, X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and superconducting quantum interference magnetometer, and tested in separation of Au(III) ions from aqueous solutions. The data for Au(III) adsorption on Fe₃O₄/SiO₂-SH are analyzed with the Langmuir, Freundlich, Temkin, and Dubinin–Radushkevich isotherm models, and the pseudo-first-order, pseudo-second-order, and intraparticle diffusion kinetics models. The adsorption behaviors of Au(III) on Fe₃O₄/SiO₂-SH follow the Langmuir isotherm model, and the adsorption process conforms to the pseudo-second-order kinetic model. The maximum adsorption capacity of Au(III) on Fe₃O₄/SiO₂-SH is 43.7 mg g^–1. Acetate anions play an important role yet Cu(II) ions have little interference in the adsorption of Au(III) on the adsorbent. A satisfactory recovery percentage of 89.5% is acquired by using an eluent with 1 M thiourea and 5% HCl, although thiols have a high affinity to Au(III) ions based on the hard-soft acid-base (HSAB) theory by Pearson.     

Carbon-coated Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> nanoparticles with surface amido groups for magnetic solid phase extraction of Cr(III), Co(II), Cd(II), Zn(II) and Pb(II) prior to their quantitation by ICP-MS

A magnetic nanosorbent was prepared from Fe₃O₄ nanoparticles and polyacrylamide using a solvothermal process. Two functions are achieved simultaneously in this process: The first consists in the formation of a carbon layer around the Fe₃O₄ nanoparticles, and the second one in the functionalization with an amido group. This combination allows the protection of Fe₃O₄ nanoparticles from dissolution in acid medium during heavy metal adsorption. The adsorbent was characterized by SEM, TEM, EDS, FTIR, TGA, and in terms of surface area. Results showed the Fe₃O₄ nanoparticles to be embedded in a sheet of carbon with folded surfaces which is functionalized with amido groups. The nanosorbent was applied to the enrichment of Cr(III), Co(II), Cd(II), Zn(II) and Pb(II) via magnetic solid phase extraction (mag-SPE). The effects of pH value, eluent type and sample volume were optimized. The validation of the procedure was verified by the analysis of a wheat gluten certified reference material (8418). The limits of detection for the above ions range from 1 to 110 ng L^?1. The relative standard deviations are <10%. The procedure was successfully applied to the enrichment of Cr(III), Co(II), Cd(II), Zn(II) and Pb(II) from various water and food samples.

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Graphical abstract Schematic of a new magnetic nanosorbent synthesized from Fe₃O₄ nanoparticles and polyacrylamide using a solvothermal method. The sorbent was used for the enrichment of Cr(III), Co(II), Cd(II), Zn(II) and Pb(II) in water and food samples for their ICP-MS detection.

     

Fast removal and determination of doxycycline in water samples and honey by Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> magnetic nanoparticles

Adsorption characteristics and doxycycline (DC) removal efficiency of Fe₃O₄ magnetic nanoparticles as adsorbents have been determined by investigating the effects of pH, concentration of the DC, amount of adsorbents, contact time, ionic strength and temperature. The mechanism of adsorption was also studied. The adsorption of DC to the Fe₃O₄ magnetic nanoparticles could be described by Langmuir-type adsorption isotherms. Short contact time between the reagents, reusability of Fe₃O₄ for three times after recycling of the nanoparticles, good precision and accuracy, wide working pH range and high breakthrough volume are among the highlights of this procedure. The proposed extraction and determination procedure based on magnetic nanoparticles as adsorbent was successfully applied to the determination of DC spiked in honey and various water samples. The method presented here is fast, simple, cheap and robust, and it does not require the use of organic solvents. Also, the method needs only a magnet and can be performed in any laboratory without sophisticated equipment.     

One-Pot Synthesis of Novel Amino-Functionalized Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> Hybrid Microspheres for Cu(II) Removal from Aqueous Solutions

In this work, we report the development of novel amino-functionalized Fe₃O₄ hybrid microspheres adsorbent from a facial and one-step solvothermal route by using FeCl₃·6H₂O as a single iron source and 3-aminophenoxy-phthalonitrile as ource of amino groups. During solvothermal process, the nitrile groups of 3-aminophenoxy-phthalonitrile would bond with the Fe₃O₄ through the phthalocyanine cyclization reaction to form the amino-functionalized Fe₃O₄ magnetic nano-material, which was confirmed by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and thermo-gravimetric analyzer (TGA). From the scanning electron microscope (SEM) and transmission electron microscopy (TEM) observation, the resulting monodispersed amino-functionalized Fe₃O₄ hybrid microspheres with the diameters of 180–200 nm were synthesized via the self-assembly process. More importantly, as-prepared Fe₃O₄ nano-materials with abundant amino groups exhibited high separation efficiency when they were used to remove the Cu(II) from aqueous solutions. Furthermore, the adsorption isotherms of Fe₃O₄ nano-material for Cu(II) removal fitted the Langmuir isotherm model, in which the calculated maximum adsorption capacity could increase from 5.51 to 16.25 mg g^–1 at room temperature. This work demonstrated that the amino-functionalized Fe₃O₄ magnetic nano-materials were promising as efficient adsorbents for the removal of heavy metal ions from wastewater in low concentration.     

Nanoparticles of type Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>-SiO<Subscript>2</Subscript>-graphene oxide and coated with an amino acid-derived ionic liquid for extraction of Al(III), Cr(III), Cu(II), Pb(II) prior to their determination by ICP-OES

An amino acid derived ionic liquid, Fe₃O₄ nanoparticles and graphene oxide (GO) were used to prepare a material for the magnetic solid phase extraction (MSPE) of the ions Al(III), Cr(III), Cu(II) and Pb(II). The material was characterized by Fourier transform infrared spectral (FT-IR), scanning electron microscopy (SEM), thermal gravimetric analysis (TGA), magnetic analysis and isoelectric point (pI) analysis. It is shown to be a viable sorbent for the separation of these metal ions. Single factor experiments were carried out to optimize adsorption including pH values, ionic strength, temperature and solution volume. Following desorption with 0.1 M HCl, the ions were quantified by inductively coupled plasma optical emission spectrometry. Under the optimum conditions, the method provides a linear range from 10 to 170 μg· L^?1 for Al(III); from 4.0 to 200 μg· L^?1 for Cr(III); from 5.0 to 170 μg· L^?1 for Cu(II); and from 5.0 to 200 μg· L^?1 for Pb(II). The limits of detection (LOD) are 6.2 ng L^?1 for Al(III); 1.6 ng L^?1 for Cr(III); 0.52 ng L^?1 for Cu(II); and 30 ng L^?1 for Pb(II). Method performance was investigated by determination of these ions in (spiked) environmental water and gave recoveries in the range of 89.1%–117.8%.

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Graphical abstract The graph shows that Al(III), Cr(III), Cu(II), Pb(II) are not adsorbed quantitatively by Fe₃O₄-SiO₂. On the other hand, Cr(III) and Pb(II) are adsorbed quantitatively by Fe₃O₄-SiO₂-GO while Al(III) and Cu(II) are not quantitatively retained. However, 3D–Fe₃O₄-SiO₂-GO-AAIL adsorb all these 4 metal ions quantitatively.

     

Mercaptobenzothiazole-functionalized magnetic carbon nanospheres of type Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@SiO<Subscript>2</Subscript>@C for the preconcentration of nickel,copper and lead prior to their determination by ICP-MS

The authors describe double-shell magnetic nanoparticles functionalized with 2-mercaptobenzothiazole (MBT) to give nanospheres of the type MBT-Fe₃O₄@SiO₂@C). These are shown to be viable and acid-resistant adsorbents for magnetic separation of the heavy metal ions Ni(II), Cu(II) and Pb(II). MBT act as a binding reagent, and the carbon shell and the silica shell protect the magnetic core. Following 12 min incubation, the loaded nanospheres are magnetically separated, the ions are eluted with 2 M nitric acid and then determined by inductively coupled plasma-mass spectroscopy. The limits of detection of this method are 2, 82 and 103 ng L￣¹ for Ni(II), Cu(II), and Pb(II) ions, respectively, and the relative standard deviations (for n = 7) are 6, 7.8, and 7.4 %. The protocol is successfully applied to the quantitation of these ions in tap water and food samples (mint, cabbage, potato, peas). Recoveries from spiked water samples ranged from 97 to 100 %.

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Graphical abstract Mercaptobenzothiazole-functionalized magnetic carbon nanospheres of type Fe₃O₄@SiO₂@C were synthesized. Then applied for magnetic solid phase extraction of Ni(II), Cu(II) and Pb(II) from water and food samples with LOD of 0.002, 0.082 and 0.103 μg L^?1 respectively.

     

Magnetite nanoparticles for removal of heavy metals from aqueous solutions: synthesis and characterization

Fe₃O₄ magnetic nanoparticles were synthesized by co-precipitation method. The structural characterization showed an average nanoparticle size of 8 nm. The synthesized Fe₃O₄ nanoparticles were tested for the treatment of synthetic aqueous solutions contaminated by metal ions, i.e. Pb(II), Cu(II), Zn(II) and Mn(II). Experimental results show that the adsorption capacity of Fe₃O₄ nanoparticles is maximum for Pb(II) and minimum for Mn(II), likely due to a different electrostatic attraction between heavy metal cations and negatively charged adsorption sites, mainly related to the hydrated ionic radii of the investigated heavy metals. Various factors influencing the adsorption of metal ions, e.g., pH, temperature, and contacting time were investigated to optimize the operating condition for the use of Fe₃O₄ nanoparticles as adsorbent. The experimental results indicated that the adsorption is strongly influenced by pH and temperature, the effect depending on the different metal ion considered.     

Comparison of Cadmium Cd2+ and Lead Pb2+ Binding by Fe2O3@SiO2‐EDTA Nanoparticles – Binding Stability and Kinetic Studies

This study describes the synthesis and characterization of ethylenediaminetetraacetic acid (EDTA) functionalized magnetic nanoparticles of 20 nm in size – Fe₃O₄@SiO₂‐EDTA – which were used as a novel magnetic adsorbent for Cd(II) and Pb(II) binding in aqueous medium. These nanoparticles were obtained in two‐stage synthesis: covering by tetraethyl orthosilicate and functionalization with EDTA derivatives. Nanoparticles were characterized using TEM, FT‐IR, and XPS methods. Metal ions were detected under optimized experimental conditions using Differential Pulse Anodic Stripping Voltammetry (DPASV) and Hanging Mercury Drop Electrode (HDME) techniques. We compared the ability of Fe₃O₄@SiO₂‐EDTA to bind cadmium and lead in concentration of 553.9 μg L^?1 and 647.5 μg L^?1, respectively. Obtained results show that the adsorption rate of cadmium binding was very high. The equilibrium for Fe₃O₄@SiO₂‐EDTA‐Cd(II) was reached within 19 min while for the Fe₃O₄@SiO₂‐EDTA‐Pb(II) was reached within 25 minutes. About 2 mg of nanoparticles was enough to bind 87.5 % Cd(II) and 54.1 % Pb(II) content. In the next step the binding capacity of Fe₃O₄@SiO₂‐EDTA nanoparticles was determined. Only 1.265 mg of Fe₃O₄@SiO₂‐EDTA was enough to bind 96.14 % cadmium ions while 5.080 mg of nanoparticles bound 40.83 % lead ions. This phenomenon proves that the studied nanoparticles bind Cd(II) much better than Pb(II). The cadmium ions binding capacity of Fe₃O₄@SiO₂‐EDTA nanoparticles decreased during storage in 0.5 M KCl solution. Two days of Fe₃O₄@SiO₂‐EDTA storage in KCl solution caused the 32 % increase in the amount of nanoparticles required to bind 60 % of cadmium while eight‐days storage caused further increase to 328 %. The performed experiment confirmed that the storage of nanoparticles in solution without any surfactants reduced their binding capacity. The best binding capacity was observed for the nanoparticles prepared directly before the electrochemical measurements.     

Adsorption behavior of <Superscript>99</Superscript>Tc on Fe,Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> and Fe<Subscript>2</Subscript>O<Subscript>4</Subscript>

Summary The adsorption of ⁹⁹Tc on the adsorbers Fe, Fe₂O₃ and Fe₃O₄ was studied by batch experiments under aerobic and anoxic conditions. The effects of pH and CO₃^2- concentration of the simulated ground water on the adsorption ratios were also investigated, and the valences of Tc in solution after the adsorption equilibrium were studied by solvent extraction. The adsorption isotherms of TcO₄- on the adsorbers Fe, Fe₂O₃ and Fe₃O₄ were determined. Experimental results have shown that the adsorption ratio of Tc on Fe decreases with the increase of pH in the range of 5-12 and increases with the decrease of the CO₃^2- concentration in the range of 10^-8M-10^-2M. Under aerobic conditions, the adsorption ratios of ⁹⁹Tc on Fe₂O₃ and Fe₃O₄ were not influenced by pH and CO₃^2-concentration. When Fe was used as adsorbent, Tc existed mainly in the form of Tc(IV) after equilibrium and in the form of Tc(VII) when the adsorbent was Fe₂O₃ or Fe₃O₄ under aerobic conditions. The adsorption ratios of Tc on Fe, Fe₂O₃ and Fe₃O₄ decreased with the increase of pH in the range of 5-12 and increased with the decrease of the CO₃^2- concentration in the range of 10^-8M-10^-2M under anoxic conditions. Tc existed mainly in the form of Tc(IV) after equilibrium when Fe, Fe₂O₃ and Fe₃O₄ was the adsorbent under anoxic conditions. The adsorption isotherms of TcO_4- on the adsorbers Fe, Fe₂O₃ and Fe₃O₄ are fairly in agreement with the Freundlich’s equation under both aerobic and anoxic conditions.     

Preparation and adsorption of magnetic Co<Subscript>0.5</Subscript>Ni<Subscript>0.5</Subscript>Fe<Subscript>2</Subscript>O<Subscript>4</Subscript>-chitosan nanoparticles

In this paper, magnetic chitosan microspheres were prepared by the emulsification cross-linking technique, with glutaraldehyde as the cross-linking agent, liquid paraffin as the dispersant, and the Span-80 as emulsifier. The time of cross-linking and the ratio of Co_0.5Ni_0.5Fe₂O₄/chitosan were investigated. The morphology was studied by different instruments. The adsorption performance was investigated and the effects of initial concentration of methyl orange, the time of cross-linking, and the amount of adsorbent were discussed. It is found that the product has uniform morphology when the ratio of magnetic Co_0.5Ni_0.5Fe₂O₄/chitosan is 1 : 2 and the time of cross-linking is 5 h; At room temperature, magnetic Co_0.5Ni_0.5Fe₂O₄–chitosan has a good adsorption toward methyl orange when the magnetic Co_0.5Ni_0.5Fe₂O₄/chitosan dosage is 20 mg.     

Preparation of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>-C18 nano-magnetic composite materials and their cleanup properties for organophosphorous pesticides

Magnetic Fe₃O₄-C18 composite nanoparticles of approximately 5–10 nm in size were synthesized and characterized by IR spectroscopy, atomic absorption spectroscopy, X-ray diffraction, and transmission electron microscopy. The magnetic Fe₃O₄-C18 composite nanoparticles were applied for cleanup and enrichment of organophosphorous pesticides. Comparative studies were carried out between magnetic Fe₃O₄-C18 composite nanoparticles and common C18 materials. Residues of organophosphorous pesticides were determined by gas chromatography in combination with a nitrogen/phosphorus detector. The cleanup and enrichment properties of magnetic Fe₃O₄-C18 composite nanoparticles are comparable with those of common C18 materials for enrichment of organophosphorous pesticides, but the cleanup and enrichment are faster and easier to perform. Figure Presumed mechanism for the adhesion of the OPs to the Fe₃O₄-C18 magnetic nanoparticles     

Synthesis of hybrid nanoparticles based on magnetic Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> nanoparticles and luminescent CdS nanoparticles

A new approach to the synthesis of hybrid nanoparticles based on magnetic Fe₃O₄ nanoparticles and CdS quantum dots, combining magnetic and luminescence properties, has been suggested. Conditions for preparation of their stable aqueous suspensions have been found, and their optical properties have been studied. Nanocomposites produced at the molar ratio Fe₃O₄: CdS = 5: 1, which exhibited the luminescence properties) and gave stable aqueous suspensions, have turned out to be most promising. The results are evidence that the synthesized nanoparticles can be used for the development of visualizing agents for in vitro biomedical research.     

Improving Pullulanase Catalysis via Reversible Immobilization on Modified Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@Polydopamine Nanoparticles

To improve the catalysis of pullulanase from Anoxybacillus sp.WB42, Fe₃O₄@polydopamine nanoparticles (Fe₃O₄@PDA) were prepared and modified with functional groups for immobilization of pullulanases via covalent binding or ionic adsorption. Immobilized pullulanases had lower thermal stability than that of free pullulanase, whereas their catalysis depended on the surface characteristics of nanoparticles. As for covalent immobilization of pullulanases onto Fe₃O₄@PDA derivatives, the spacer grafted onto Fe₃O₄@PDA made the catalytic efficiency of pullulanase increase up to the equivalence of free enzyme but dramatically reduced the pullulanase thermostability. In contrast, pullulanases bounded ionically to Fe₃O₄@PDA derivatives had higher activity recovery and catalytic efficiency, and their catalytic behaviors varied with the modifier grafted onto Fe₃O₄@PDA. Among these immobilized pullulanases, ionic adsorption of pullulanase on Fe₃O₄@PDA-polyethyleneimine-glycidyltrimethylammonium gave a high-performance and durable catalyst, which displayed not only 1.5-fold increase in catalytic efficiency compared to free enzyme but also a significant improvement in operation stability with a half of initial activity after 27 consecutive cycles with a total reaction time of 13.5 h, and was reversible, making this nanoparticle reusable for immobilization.     

Catalytic Properties of TiO<Subscript>2</Subscript>/Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> Nanoparticles in Plasma Chemical Treatment

We proposed here a new process coupling dielectric barrier discharge (DBD) plasma with magnetic photocatalytic material nanoparticles for improving yield in DBD degradation of methyl orange (MO). TiO₂ doped Fe₃O₄ (TiO₂/Fe₃O₄) was prepared by the sol-gel method and used as a new type of magnetic photocatalyst in DBD system. It was found that the introduction of TiO₂/Fe₃O₄ in DBD system could effectively make use of the energy generated in DBD process and improve hydroxyl radical contributed by the main surface Fenton reaction, photocatalytic reaction and catalytic decomposition of dissolved ozone. Most part of MO (88%) was degraded during 30 min at peak voltage of 13 kV and TiO₂/Fe₃O₄ load of 100 mg/L, with a rate constant of 0.0731 min^?1 and a degradation yield of 7.23 g/(kW h). The coupled system showed higher degradation efficiency for MO removal.     

Study of magnetic ferrite nanoparticles labeled with <Superscript>99m</Superscript>Tc-pertechnetate

This study examined the applications of novel non-polymer magnetic ferrite nanoparticles (Fe₃O₄ NPs) labeled with ^99mTc-pertechnetate (^99mTcO₄ ⁻). The radiochemistry, chemistry, and biodistribution of Fe₃O₄ NPs labeled with ^9mTcO₄ ⁻ were analyzed. This paper employed instant thin layer chromatography and magnetic adsorption to evaluate the labeling efficiency and stability of ^99mTc-Fe₃O₄ at various reaction conditions. A scanning electron microscope, X-ray diffractometer, Fourier transform infrared spectrometer, laser particle size analyzer, and superconducting quantum interference device magnetometer were used to analyze the physical and chemical properties of the Fe₃O₄ and ⁹⁹Tc-Fe₃O₄ nanoparticles. The biodistribution and excretion of ^99mTc-Fe₃O₄ were also investigated. Radiochemical analyses showed that the labeling efficiency was over 92% after 1 min in the presence of a reducing agent. Hydroxyl and amine groups covered the surface of the Fe₃O₄ particles. Therefore, ⁹⁹Tc (VII) reduced to lower oxidation states and might bind to Fe₃O₄ NPs. The sizes of the ⁹⁹Tc-Fe₃O₄ NPs were about 600 nm without ultrasound vibrations, and the particle sizes were reduced to 250 nm under ultrasound vibration conditions. Nonetheless, Fe₃O₄ NPs and ⁹⁹Tc-Fe₃O₄ NPs exhibited superparamagnetic properties, and the saturation magnetization values were about 55 and 47 emu/g, respectively. The biodistribution showed that a portion of the ^99mTc-Fe₃O₄ nanoparticles might embolize in a pulmonary capillary initially; the embolism radioactivity was cleared from the lungs and was then taken up by the liver. ^99mTc-Fe₃O₄ metabolized very slowly only 1–2% of the injected dose (ID) was excreted in urine and about 2.37% ID/g was retained in the liver 4 h after injection. Radiopharmaceutically, ^99mTc-Fe₃O₄ NPs displayed long-term retention, and only ^99mTc-Fe₃O₄ NPs that dissociated to free pertechnetate could be excreted in urine. This research evaluated the feasibility of non-polymer magnetic ferrite NPs labeled with technetium as potential radiopharmaceuticals in nuclear medicine.     

Rattle-type Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@SnO<Subscript>2</Subscript> core-shell nanoparticles for dispersive solid-phase extraction of mercury ions

The synthesis of rattle-type nanostructured Fe₃O₄@SnO₂ is described along with their application to dispersive solid-phase extraction of trace amounts of mercury(II) ions prior to their determination by continuous-flow cold vapor atomic absorption spectrometry. The voids present in rattle-type structures make the material an effective substrate for adsorption of Hg(II), and also warrant high loading capacity. The unique morphology, large specific surface, magnetism property and the synergistic effect of magnetic cores and SnO₂ shells render these magnetic nanorattles an attractive candidate for solid-phase extraction of heavy metal ions.The sorbent was characterized by transmission electron microscopy, scanning electron microscopy, FTIR, energy-dispersive X-ray spectroscopy and by the Brunnauer-Emmett-Teller technique. The effects of pH value, adsorption time, amount of sorbent, volume of sample solutions, concentration and volume of eluent on extraction efficiencies were evaluated. The calibration plot is linear in the 0.1 to 40 μg·L^?1 concentration range, and the preconcentration factor is 49. The detection limit is 28 ng·L^?1. The sorbent was applied to the analysis of (spiked) river and sea water samples. Recoveries ranged from 97.2 to 100.5%.

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Graphical abstract A yolk-shell structure based on a Fe₃O₄ core and SnO₂ shell was developed as an efficient MSPE sorbent. A middle silica layer was etched by alkaline solution. The resulting sorbent was utilized for preconcentration of mercury ions from aqueous media.

     

Preconcentration of Pb(II) by using Mg(II)-doped NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles as a magnetic solid phase extraction agent

Magnesium(II)-doped nickel ferrite (Mg–NiFe₂O₄) nanoparticles are introduced as a new adsorbent for magnetic solid phase extraction of lead(II) ions from aqueous solutions. The structure and morphology of the adsorbent was characterized by FTIR, X-ray diffraction and scanning electron microscopy. The effects of pH value, amount of adsorbent, type, concentration and volume of the eluent and adsorption/desorption time on the extraction efficiency were studied. Following elution with hydrochloric acid, Pb(II) ions were quantified by flame atomic absorption spectrometry. Under optimized conditions, the calibration graph is linear in the 0.5–125 ng mL^?1 Pb(II) ion concentration range. Other figures of merit include (a) a 0.2 ng mL^?1 limit of detection, (b) an enrichment factor of 200, (c) an intra-day relative standard deviation (for n =?6 at 50 ng mL^?1) of 1.6%, and (d) an inter-day precision of 3.8%. The method was validated by the analysis of the certified reference material, NIST SRM 1566b. It was successfully applied to the determination of Pb(II) ion in spiked water samples, industrial wastewater and acidic lead battery waters.

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Graphical abstract Schematic of the synthesis of Mg(II)-doped NiFeO₄ nanoparticles and their application as a magnetic sorbent for solid-phase extraction of a Pb(II) ions prior to determination by flame atomic absorption spectrometry (FAAS).

     

Photo-fenton refreshable Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@HCS adsorbent for the elimination of tetracycline hydrochloride

A yolk–shell-structured sphere composed of a superparamagnetic Fe₃O₄ core and a carbon shell (Fe₃O₄@HCS) was etched from Fe₃O₄@SiO₂@carbon by NaOH, which was synthesized through the layer-by-layer coating of Fe₃O₄. This yolk–shell composite has a shell thickness of ca. 27 nm and a high specific surface area of 213.2 m² g^?1. Its performance for the magnetic removal of tetracycline hydrochloride from water was systematically examined. A high equilibrium adsorption capacity of ca. 49.0 mg g^?1 was determined. Moreover, the adsorbent can be regenerated within 10 min through a photo-Fenton reaction. A stable adsorption capacity of 44.3 mg g^?1 with a fluctuation <10% is preserved after 5 consecutive adsorption–degradation cycles, demonstrating its promising application potential in the decontamination of sewage water polluted by antibiotics.     

In-situ growth of Co<Subscript>3</Subscript>O<Subscript>4</Subscript> nanoparticles on mesoporous carbon nanofibers: a new nanocomposite for nonenzymatic amperometric sensing of H<Subscript>2</Subscript>O<Subscript>2</Subscript>

The paper describes a nonenzymatic amperometric H₂O₂ sensor that uses a nanocomposite consisting of Co₃O₄ nanoparticles (NPs) and mesoporous carbon nanofibers (Co₃O₄-MCNFs). The Co₃O₄ NPs were grown in situ on the MCNFs by a solvothermal procedure. The synergetic combination of the electrocatalytic activity of the Co₃O₄ NPs and the electrical conductivity of MCNFs as an immobilization matrix enhance the sensing ability of the hybrid nanostructure. The oxidation current, best measured at 0.2 V (vs. SCE) is linear in the 1 to 2580 μM H₂O₂ concentration range, with a 0.5 μM lower detection limit (at an S/N ratio of 3). The sensor is highly selective even in the presence of common electroactive interferents. It was applied to the determination of H₂O₂ in spiked milk samples.

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Graphical abstract Schematic of the synthesis of a nanocomposite consisting of Co₃O₄ nanoparticles (NPs) and mesoporous carbon nanofibers (Co₃O₄-MCNFs) by a solvothermal procedure. It was used as electrocatalyst for direct oxidation of H₂O₂.