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1.
A new Fe(3)O(4)/polyaniline nanoparticle (PANI) material has been successfully developed as magnetic solid-phase extraction sorbent in dispersion mode for the determination of methylmercury (MeHg) in aqueous samples, via quantification by gas chromatography/mass spectrometry (GC-MS). The resultant core-shell magnetic solid-phase extraction nanoparticle (MSPE-NP) sorbent was characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDS) and Fourier transform-infrared (FTIR) spectroscopy. Fe(3)O(4)/PANI composites showed fibrous structure with diameters between 50 and 100 nm for fibers. The MSPE-NP process involved the dispersion of the Fe(3)O(4)/PANI nanoparticles in water samples with sonication, followed by magnetic aided retrieval of the sorbent and then, solvent (hexane) desorption of extracted MeHg for GC-MS analysis. The extraction, derivatization and adsorption conditions were optimized by selecting the appropriate extraction parameters including the amount of sorbent, extraction time, derivatizing reagent volume and extraction solvent. The calibration graph was linear in the concentration range of 0.5-300 ng mL(-1) (R(2)>0.993) with detection limit of 0.1 ng mL(-1) (n=3), while the repeatability was 4.1% (n=5). Enrichment factor was obtained as 91. Seawater sample was analyzed as real sample and good recoveries (>98%) were obtained at different spiked values.  相似文献   

2.
In this study, the superparamagnetic attapulgite/Fe3O4/polyaniline (ATP/Fe3O4/PANI) nanocomposites were successfully synthesized by a one-pot method. Fe (III) was applied as both the oxidant for the oxidative polymerization of aniline and the single iron source of Fe3O4 formed by the redox reaction between aniline and Fe (III). The ATP/Fe3O4/PANI was used as sorbent for magnetic dispersive solid phase extraction (MDSPE) of benzoylurea insecticides (BUs) in environmental water samples. The as-prepared nanocomposite sorbents were characterized by Fourier transform infrared spectra (FT-IR), X Ray diffraction (XRD), scanning electron microscopy(SEM), transmission electron microscopy (TEM), and vibrating sample magnetometry. Various experimental parameters affecting the ATP/Fe3O4/PANI-based MDSPE procedure, including the composition of the nanocomposite sorbents, amount of ATP/Fe3O4/PANI nanocomposites, vortex time, pH, and desorption conditions were investigated. Under the optimal conditions, a good linearity was observed for all target analytes, with correlation coefficients (r2) ranging from 0.9985 to 0.9997; the limits of detection (LOD) were in the range of 0.02–0.43 μg L−1, and the recoveries of analytes using the proposed method ranged between 77.37% and 103.69%. The sorbents exhibited an excellent reproducibility in the range of 1.52–5.27% in extracting the five target analytes. In addition, the intra-day and inter-day precision values were found to be in the range of 0.78–6.86% and 1.66–8.41%, respectively. Finally, the proposed ATP/Fe3O4/PANI-based MDSPE method was successfully applied to analyze river water samples by rapid preconcentration of BUs.  相似文献   

3.
Polyaniline (PANI) nanotubes containing Fe3O4 nanoparticles were synthesized under ultrasonic irradiation of the aqueous solutions of aniline, ammonium peroxydisulfate (APS), phosphoric acid (H3PO4), and the quantitative amount of Fe3O4. It was found that the obtained samples had the morphologies of nanotubes. TEM images and selected area electronic diffractions showed that Fe3O4 nanoparticles were embedded in PANI nanotubes. We thought that the mechanism of the formation of PANI/Fe3O4 nanotubes could be attributed to the ultrasonic irradiation and the H3PO4-aniline salt template. The molecular structure of PANI/Fe3O4 nanotubes were characterized by Fourier transform infrared spectroscopy (FTIR), UV-vis absorption spectra and X-ray diffraction (XRD). The conductivity and magnetic properties of the PANI nanotubes containing Fe3O4 nanoparticles were also investigated.  相似文献   

4.
Porous magnetic composites were prepared by the synthesis of molecular sieve MCM-41 in the presence of Fe3O4 nanoparticles with average diameter of 15 nm. Nanoparticles were captured by porous silica matrix MCM-41, which resulted in their incorporation, as it was confirmed by TEM, SEM and X-ray diffraction. The materials possessed high surface area (392-666 m2 g−1), high pore volume (0.39-0.73 cm3 g−1) along with high magnetic response (MS up to 28.4 emu g−1 at 300 K). Calcination of samples resulted in partial oxidation of Fe3O4 to α-Fe2O3. The influence of nanoparticles content on sorption and magnetic properties of the composites was shown. No hysteresis was found for the samples at 300 K; at 5 K, HC was in the range 370-385 G for non-calcinated samples and 350-356 G for calcinated ones.  相似文献   

5.
The carbon coated Fe3O4 nanoparticles (Fe3O4/C) were synthesized by a simple hydrothermal reaction and applied as solid-phase extraction (SPE) sorbents to extract trace polycyclic aromatic hydrocarbons (PAHs) from environmental water samples. The Fe3O4/C sorbents possess high adsorption capacity and extraction efficiency due to strong adsorption ability of carbon materials and large surface area of nanoparticles, and only 50 mg of sorbents are required to extract PAHs from 1000 mL water samples. The adsorption attains equilibrium rapidly and analytes are eluted with acetonitrile readily. Salinity and solution pH have no obvious effect on the recoveries of PAHs, which avoids fussy adjustment to water sample before extraction. Under optimized conditions, the detection limits of PAHs are in the range of 0.2–0.6 ng L−1. The accuracy of the method was evaluated by the recoveries of spiked samples. Good recoveries (76–110%) with low relative standard deviations from 0.8% to 9.7% are achieved. This new SPE method provides several advantages, such as high extraction efficiency, high breakthrough volumes, convenient extraction procedure, and short analysis times. To our knowledge, this is the first time that Fe3O4/C nanoparticles are used for the pretreatment of environmental water samples.  相似文献   

6.
In this paper, surface plasmon resonance biosensors based on magnetic core/shell Fe(3)O(4)/SiO(2) and Fe(3)O(4)/Ag/SiO(2) nanoparticles were developed for immunoassay. With Fe(3)O(4) and Fe(3)O(4)/Ag nanoparticles being used as seeding materials, Fe(3)O(4)/SiO(2) and Fe(3)O(4)/Ag/SiO(2) nanoparticles were formed by hydrolysis of tetraethyl orthosilicate. The aldehyde group functionalized magnetic nanoparticles provide organic functionality for bioconjugation. The products were characterized by scanning electronic microscopy (SEM), transmission electronic microscopy (TEM), FTIR and UV-vis absorption spectrometry. The magnetic nanoparticles possess the unique superparamagnetism property, exceptional optical properties and good compatibilities, and could be used as immobilization matrix for goat anti-rabbit IgG. The magnetic nanoparticles can be easily immobilized on the surface of SPR biosensor chip by a magnetic pillar. The effects of Fe(3)O(4)/SiO(2) and Fe(3)O(4)/Ag/SiO(2) nanoparticles on the sensitivity of SPR biosensors were also investigated. As a result, the SPR biosensors based on Fe(3)O(4)/SiO(2) nanoparticles and Fe(3)O(4)/Ag/SiO(2) nanoparticles exhibit a response for rabbit IgG in the concentration range of 1.25-20.00 μg ml(-1) and 0.30-20.00 μg ml(-1), respectively.  相似文献   

7.
This work describes a magnetic Fe3O4/graphene oxide (GO)-based solid-phase extraction (MSPE) technique for high performance liquid chromatography (HPLC) detection of malachite green (MG) and crystal violet (CV) in environmental water samples. Fe3O4/ GO magnetic nanoparticles were synthesised by a chemical co-precipitation method and characterised by scanning electron micrograph, transmission electron microscope, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and surface area analyser. The prepared Fe3O4/GO magnetic nanoparticles were used as the adsorbents of MSPE for MG and CV. By coupling with HPLC, a sensitive and cost-effective method for simultaneous determination of MG and CV was developed. The important parameters including the amount of Fe3O4/GO, pH of the sample solution, extraction time, salt effect, the type and volume of desorption solvent were investigated in detail. Under optimised conditions, the calibration curves were linear in the concentration range of 0.5–200 μg L?1, and the limits of detection were 0.091 and 0.12 μg L?1 for MG and CV, respectively. Finally, the established MSPE-HPLC method was successfully applied to determine MG and CV in environmental water samples with the recoveries ranging from 91.5% to116.7%.  相似文献   

8.
Polythiophene (PT) was used as a surface modifier of graphene/Fe3O4 (G/Fe3O4) composite to increase merit of it, and also overcome some limitations and disadvantages of using G/Fe3O4 alone as solid phase extraction (SPE) sorbent. An in-situ chemical polymerization method was employed to prepare G/Fe3O4@PT nanocomposites. Application of this newly designed material in the magnetic SPE (MSPE) of polycyclic aromatic hydrocarbons (PAHs), as model analytes, in the environmental water samples was investigated. The characterization of the hybrid material was performed using transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray analysis, Fourier transform-infrared (FT-IR) spectroscopy and vibrating sample magnetometry. Seven important parameters, affecting the extraction efficiency of PAHs, including: amount of adsorbent, adsorption and desorption times, type and volume of the eluent solvent, initial sample volume and salt content of the sample were evaluated. The optimum extraction conditions were obtained as: 4 min for extraction time, 20 mg for sorbent amount, 100 mL for initial sample volume, toluene as desorption solvent, 0.6 mL for desorption solvent volume, 6 min for desorption time and 30% (w/v) for NaCl concentration. Good performance data were obtained at the optimized conditions. Detection limits were in the range of 0.009–0.020 μg L−1 in the real matrix. The calibration curves were linear over the concentration ranges from 0.03 to 80 μg L−1 with correlation coefficients (R2) between 0.995 and 0.998 for all the analytes. Relative standard deviations were ranged from 4.3 to 6.3%. Appropriate recovery values, in the range of 83–107%, were also obtained for the real sample analysis.  相似文献   

9.
Cui YR  Hong C  Zhou YL  Li Y  Gao XM  Zhang XX 《Talanta》2011,85(3):1246-1252
Orientedly bioconjugated core/shell Fe3O4@Au magnetic nanoparticles were synthesized for cell separation. The Fe3O4@Au magnetic nanoparticles were synthesized by reducing HAuCl4 on the surfaces of Fe3O4 nanoparticles, which were further characterized in detail by TEM, XRD and UV-vis spectra. Anti-CD3 monoclonal antibody was orientedly bioconjugated to the surface of Fe3O4@Au nanoparticles through affinity binding between the Fc portion of the antibody and protein A that covalently immobilized on the nanoparticles. The oriented immobilization method was performed to compare its efficiency for cell separation with the non-oriented one, in which the antibody was directly immobilized onto the carboxylated nanoparticle surface. Results showed that the orientedly bioconjugated Fe3O4@Au MNPs successfully pulled down CD3+ T cells from the whole splenocytes with high efficiency of up to 98.4%, showing a more effective cell-capture nanostructure than that obtained by non-oriented strategy. This developed strategy for the synthesis and oriented bioconjugation of Fe3O4@Au MNPs provides an efficient tool for cell separation, and may be further applied to various fields of bioanalytical chemistry for diagnosis, affinity extraction and biosensor.  相似文献   

10.
A novel amperometric immunosensor was developed by immobilizing ferritin antibody (FeAb) on the surface of Fe3O4 magnetic nanoparticles/chitosan composite film modified glassy carbon electrode (GCE). This material combined the advantages of inorganic Fe3O4 nanoparticles with the organic polymer chitosan. The stepwise assembly procedure of the immunosensor was characterized by means of differential pulse voltammetry (DPV) and ac impedance. The K3Fe(CN)6/K4Fe(CN)6 was used as a marker to probe the interface and to determinate ferritin. The factors that could influence the performance of the resulting immunosensor were studied in detail. After the immunosensor was incubated with ferritin for 32 min at 35 °C, the DPV current decreased linearly with the logarithm of ferritin concentration in the range from 20 to 500 ng mL−1 with a correlation coefficient of 0.995 and a detection limit of 7.0 ng mL−1. This immunosensor was used to analyze ferritin in human serum samples. The analytical results showed that the developed immunoassay was comparable with the radioimmunoassay (RIA), and the studied immunosensor exhibited good accuracy, high sensitivity, and long-term stability for 3 weeks, which implies a promising alternative approach for detecting ferritin in clinical diagnosis.  相似文献   

11.
A new method based on the combination of magnetic solid phase extraction (MSPE) and spectrofluorimetric determination was developed for isolation and preconcentration of fluoxetine form aquatic and biological samples using sodium dodecyl sulfate (SDS) coated Fe3O4 nanoparticles (NPs) as a sorbent. The unique properties of Fe3O4 NPs including high surface area and strong magnetism were utilized effectively in the MSPE process. Effect of different parameters influencing the extraction efficiency of fluoxetine including the amount of Fe3O4 and SDS, pH value, sample volume, extraction time, desorption solvent and time were optimized. Under optimized condition, the method was successfully applied to the extraction of fluoxetine from water and urine samples and absolute recovery amount of 85%, detection limit of 20 μg L−1 and a relative standard deviation (RSD) of 1.4% were obtained. The method linear response was over a range of 50–1000 μg L−1 with R2 = 0.9968. The relative recovery in different aquatic and urine matrices were investigated and values of 80% to 104% were obtained. The whole procedure showed to be conveniently fast, efficient and economical for extraction of fluoxetine from environmental and biological samples.  相似文献   

12.
In this paper, 1-hexadecyl-3-methylimidazolium bromide (C16mimBr)-coated Fe3O4 magnetic nanoparticles (NPs) as an adsorbent of mixed hemimicelles solid-phase extraction was investigated for the preconcentration of two chlorophenols (CPs) in environmental water samples prior to HPLC with UV detection at 285 nm. The high surface area and excellent adsorption capacity of the Fe3O4 NPs after modification with C16mimBr were utilized adequately in the SPE process. By the rapid isolation of Fe3O4 NPs through placing a strong magnet on the bottom of beaker, the time-consuming preconcentration process of loading large volume sample in conventional SPE method with a column can be avoided. A comprehensive study of the adsorption conditions such as the zeta-potential of Fe3O4 NPs, added amounts of C16mimBr, pH value, standing time and maximal extraction volume were also presented. Under optimized conditions, two analytes of 2,4-dichlorophenol (2,4-DCP) and 2,4,6-trichlorophenol (2,4,6-TCP) were quantitatively determined. The method was then used to determine the two CPs in real environmental water samples. The accuracy of method was evaluated by recovery measurements on spiked samples. Good recovery results (74–90%) were achieved. It is important to note that satisfactory preconcentration factors and extraction recoveries for the two CPs were obtained with only a small amount of Fe3O4 NPs (40 mg) and C16mimBr (24 mg).  相似文献   

13.
Magnetic Fe3O4 nanoparticles as a heterogeneous catalyst, were found to be efficient for the synthesis of a series of pyranopyrazoles by a four component reaction of a mixture of hydrazine hydrate, ethyl acetoacetate, aldehydes/ketones and malononitrile in water at room temperature. The products were attributed to the nanosize of about 16 nm in which the catalyst could act as a nanoreactor. The present protocol offers the advantages of clean reaction, short reaction time, high yield, easy purification and economic availability of the catalyst.  相似文献   

14.
In-tube magnetic solid phase microextraction (in-tube MSPME) of fluoroquinolones from water and urine samples based on the use of sodium dodecyl sulfate (SDS) coated Fe3O4 nanoparticles packed tube has been reported. After the preparation of Fe3O4 nanoparticles (NPs) by a batch synthesis, these NPs were introduced into a stainless steel tube by a syringe and then a strong magnet was placed around the tube, so that the Fe3O4 NPs were remained in the tube and the tube was used in the in-tube SPME-HPLC/UV for the analysis of fluoroquinolones in water and urine samples. Plackett–Burman design was employed for screening the variables significantly affecting the extraction efficiency. Then, the significant factors were more investigated by Box–Behnken design. Calibration curves were linear (R2 > 0.990) in the range of 0.1–1000 μg L−1 for ciprofloxacin (CIP) and 0.5–500 μg L−1 for enrofloxacin (ENR) and ofloxacin (OFL), respectively. LODs for all studied fluoroquinolones ranged from 0.01 to 0.05 μg L−1. The main advantages of this method were rapid and easy automation and analysis, short extraction time, high sensitivity, possibility of fully sorbent collection after analysis, wide linear range and no need to organic solvents in extraction.  相似文献   

15.
In this work, a magnetic solid-phase extraction protocol followed with high-performance liquid chromatography analysis was developed for the determination of maltol and ethyl maltol in food samples. The Fe3O4 nanoparticles were prepared by one-step hydrothermal method and was used as adsorbent for clean and preconcentrated maltol and ethyl maltol in food samples. The as-prepared Fe3O4 nanoparticle was characterized by transmission electron microscope, Fourier transform infrared spectroscopy, X-ray diffraction, and vibrating sample magnetometer. The extraction conditions including the amount of material, extraction time, pH, temperature, and desorption solvents were investigated, respectively. Under the optimized conditions, the detection limits of 0.04 and 0.05?µg?mL?1 could be achieved for maltol and ethyl maltol. The recoveries between 84.2 and 103.4% with RSDs lower than 2.30% were obtained for the analysis of spiked plum candy sample. The developed method was successfully applied to the analysis of real samples, such as juice, chocolate, and plum candy.  相似文献   

16.
In this paper, monodisperse Fe3O4 nanoparticles with single crystalline structure were synthesized via a facile environment-friendly method. And the size of the nanoparticles ranges from 10 nm to 15 nm. As-synthesized Fe3O4 were characterized by X-ray diffraction instrument (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FT-IR) spectrometer and field emission transmission electron microscope (FE-TEM). The effect of tartaric acid (TA) amount on products was investigated by XRD and TEM. The results indicated that TA could commendably modulate the crystalline phase, morphology and size of nanometer Fe3O4. A possible generated mechanism of Fe3O4 crystals was proposed in virtue of UV–vis absorption spectra. Besides, the magnetic properties of as-synthesized Fe3O4 were detected.  相似文献   

17.
A novel, facile and inexpensive solid phase extraction (SPE) method using ethylene glycol bis-mercaptoacetate modified 3-(trimethoxysilyl)-1-propanethiol grafted Fe3O4 nanoparticles coupled with spectrofluorimetric detection was proposed for determination of aflatoxin M1 (AFM1) in liquid milk samples. The method uses the advantage fluorescence enhancement by β-cyclodexterin complexation of AFM1 in 12% (v/v) acetonitrile–water and the remarkable properties of Fe3O4 nanoparticles namely high surface area and strong magnetization were utilized to achieve high enrichment factor (57) and satisfactory extraction recoveries (91–102%) using only 100 mg of magnetic adsorbent. Furthermore, fast separation time of about 15 min avoids many time-consuming column-passing procedures of conventional SPE. The main factors affecting extraction efficiency including pH value, desorption conditions, extraction/desorption time, sample volume, and adsorbent amount were evaluated and optimized. Under the optimal conditions, a wide linear range of 0.04–8 ng mL−1 with a low detection limit of 0.015 ng mL−1 was obtained. The developed method was applied for extraction and preconcentration of AFM1 in three commercially available milk samples and the results were compared with the official AOAC method.  相似文献   

18.
A novel Fe3O4–poly(aniline-naphthylamine)-based nanocomposite was synthesized by chemical oxidative polymerization process as a magnetic sorbent for micro solid phase extraction. The scanning electron microscopy images of the synthesized nanocomposite revealed that the copolymer posses a porous structure with diameters less than 50 nm. The extraction efficiency of this sorbent was examined by isolation of rhodamine B, a mutagenic and carcinogenic dye, from aquatic media in dispersion mode. Among different synthesized polymers, Fe3O4/poly(aniline-naphthylamine) nanocomposite showed a prominent efficiency. Parameters including the desorption solvent, amount of sorbent, desorption time, sample pH, ionic strength, extraction time and stirring rate were optimized. Under the optimum condition, a linear spiked calibration curve in the range of 0.35–5.00 μg L−1 with R2 = 0.9991 was obtained. The limits of detection (3Sb) and limits of quantification (10Sb) of the method were 0.10 μg L−1 and 0.35 μg L−1 (n = 3), respectively. The relative standard deviation for water sample with 0.5 μg L−1 of RhB was 4.2% (n = 5) and the absolute recovery was 92%. The method was applied for the determination of rhodamine B in dishwashing foam, dishwashing liquid, shampoo, pencil, matches tips and eye shadows samples and the relative recovery percentage were in the range of 94–99%.  相似文献   

19.
A facile method of fabricating novel heat-generating membranes composed of electrospun polyurethane (PU) nanofibers decorated with superparamagnetic iron oxide nanoparticles (NPs) is reported. Electrospinning was used to produce polymeric nanofibrous matrix, whereas polyol immersion technique allowed in situ assembly of well-dispersed Fe3O4 NPs on the nanofibrous membranes without any surfactant, and without sensitizing and stabilizing reagent. The assembly phenomena can be explained by the hydrogen-bonding interactions between the amide groups in the PU matrix and the hydroxyl groups capped on the surface of the Fe3O4 NPs. The prepared nanocomposite fibers showed acceptable magnetization value of 33.12 emu/g, after measuring the magnetic hysteresis loops using SQUID. Moreover, the inductive heating property of electrospun magnetic nanofibrous membranes under an alternating current (AC) magnetic field was investigated. We observed a progressive increase in the heating rate with the increase in the amount of magnetic Fe3O4 NPs in/on the membranes. The present electrospun magnetic nanofibrous membrane may be a potential candidate as a novel heat-generating substrate for localized hyperthermia cancer therapy.  相似文献   

20.
设计并合成了一种以磁性纳米粒子为核,聚合物为中间层,金属有机骨架材料为外层的三层结构磁性复合材料(Fe3O4@PAA@ZIF 8)。首先利用溶剂热法制备Fe3O4纳米粒子,然后通过蒸馏沉淀聚合法在Fe3O4纳米粒子表面包覆聚丙烯酸(PAA)层,最后通过原位沉积法在PAA外部包覆ZIF 8。在对Fe3O4@PAA@ZIF 8的组成和结构进行表征的基础上,深入研究其对孔雀石绿(MG)的吸附性能。透射电子显微镜(TEM)显示 Fe3O4@PAA@ZIF 8 具有明显的三层结构,Fe3O4的平均粒径为 117nm,PAA 层厚度约为 17 nm,ZIF 8层的厚度约为 14 nm。Fe3O4@PAA@ZIF 8对 MG 的吸附量随着 pH 的升高而增大,吸附过程符合准二阶动力学模型和 Langmuir等温吸附模型。此外,Fe3O4@PAA@ZIF 8还表现出良好的重复利用性能,8次循环利用后对MG(500 mg·L-1)的最大吸附量仍可达982 mg·g-1。  相似文献   

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