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1.
An extracting medium based on chitosan–polypyrrole (CS–PPy) magnetic nanocomposite was synthesized by chemical polymerization of pyrrole at the presence of chitosan magnetic nanoparticles (CS-MNPs) for micro-solid phase extraction. In this work, magnetic nanoparticles, the modified CS-MNPs and different types of CS–PPy magnetic nanocomposites were synthesized. Extraction efficiency of the CS–PPy magnetic nanocomposite was compared with the CS-MNPs and Fe3O4 nanoparticles for the determination of naproxen in aqueous samples, via quantification by spectrofluorimetry. The scanning electron microscopy images obtained from all the prepared nanocomposites revealed that the CS–PPy magnetic nanocomposite possess more porous structure. Among different synthesized magnetic nanocomposites, CS–PPy magnetic nanocomposite showed a prominent efficiency. Influencing parameters on the morphology of CS–PPy magnetic nanocomposite such as weight ratio of components was also assayed. In addition, effects of different parameters influencing the extraction efficiency of naproxen including desorption solvent, desorption time, amount of sorbent, ionic strength, sample pH and extraction time were investigated and optimized. Under the optimum condition, a linear calibration curve in the range of 0.04–10 μg mL−1 (R2 = 0.9996) was obtained. The limits of detection (3Sb) and limits of quantification (10Sb) of the method were 0.015 and 0.04 μg mL−1 (n = 3), respectively. The relative standard deviation for water sample spiked with 0.1 μg mL−1 of naproxen was 3% (n = 5) and the absolute recovery was 92%. The applicability of method was extended to the determination of naproxen in tap water, human urine and plasma samples. The relative recovery percentages for these samples were in the range of 56–99%.  相似文献   

2.
A novel core-shell sphere with controlled shell thickness was synthesized by in situ chemical oxidative polymerization of pyrrole on FTS (Fe2O3/TiO2/SiO2 composite) surface. The dual porosity of 2-3 nm and 40-50 nm in FTS core particle provides the hybrids with a high surface area to volume ratio, which enormously facilitates the molecule diffusion process. Furthermore, the porous FTS particle encapsulate Fe2O3 and TiO2 leading to its synergetic interaction with the PPy coating based on FTIR analysis. The unique structure and composition of the hybrid spheres result in new sensing property that is not available from their single counterparts. Cyclic voltammetry results demonstrate that the spheres with appropriate concentration of PPy exhibit enhanced electrocatalytic activity toward the reduction of H2O2 in 0.1 M phosphate buffer solution. The sensing performance tests show that the hybrids possess good linear response in wide H2O2 concentration range (10-4000 μM) and high sensitivity to H2O2 (0.653 A M−1 cm−2) at room temperature. The formation mechanism of the spheres was proposed based on the fact that the FTS core was coated firstly by a smooth PPy layer and then PPy nanoparticles. The work reported here provides an alternative concept for preparation of functional materials with new nanostructures and properties.  相似文献   

3.
Fengna Xi 《Talanta》2009,78(3):1077-360
A simple and controllable electrodeposition approach was established for one-step construction of novel reagentless biosensors by in situ formation of chitosan-carbon nanotubes-nile blue-horseradish peroxidase (CS-CNTs-NB-HRP) biocomposite film on electrode surface. The mediator effect of NB, conducting performance of CNTs and the biocompatible microenvironment of CS were combined by such one-step non-manual process. NB could interact with CNTs and resulted in good dispersion of CNTs-NB nanocomposites in aqueous solution. Cyclic voltammetry measurements demonstrated that electrons were efficiently shuttled between HRP and the electrode mediated by NB. The developed reagentless biosensor exhibited a fast amperometric response for the determination of H2O2 and 95% of the steady-state current was obtained within 2 s. The linear response of the reagentless biosensor for the determination of H2O2 ranged from 1.0 × 10−6 to 2.4 × 10−4 mol l−1 with a detection limit of 1.2 × 10−7 mol l−1. The biosensor exhibited high reproducibility and long-time storage stability. The as-prepared biosensor also showed effective anti-interference capability. The ease of the one-step non-manual technique and the promising feature of the biocomposite could serve as a versatile platform for fabricating electrochemical biosensors.  相似文献   

4.
A label-free amperometric immunosensor for the detection of methamphetamine was developed. The prussian blue deposited/l-cystine-modified electrode was covered with nano-Au/(3-mercaptorpropyl) trime-thoxysilane film. Then, the nano-Au was used for the immunosensor platform to capture a large amount of anti-methamphetamine. PB exhibited excellent electrocatalytical properties toward the reduction of H2O2 at low overpotentia to amplify the amperometric signal, which enhanced the sensitivity of the immunosensor. The active sites of PB could be shielded and the access of H2O2 from solution to the electrode might be partially blocked after the completion of immunoassay, led to a linear decrease in the response current of the electrode over the range from 1.0 × 10−8 to 5.0 × 10−6 mol L−1of MA. The obtained immunosensor displayed excellent catalytic reduction toward H2O2 due to high activity and selectivity of PB. The influence of relevant experimental variables, including the construction of immunosensor platform, the amount of MPS and the time of immunoaction, was examined and optimized.  相似文献   

5.
Yongjin Zou  Lixian Sun  Fen Xu 《Talanta》2007,72(2):437-442
A Prussian Blue (PB)/polyaniline (PANI)/multi-walled carbon nanotubes (MWNTs) composite film was fabricated by step-by-step electrodeposition on glassy carbon electrode (GCE). The electrode prepared exhibits enhanced electrocatalytic behavior and good stability for detection of H2O2 at an applied potential of 0.0 V. The effects of MWNTs thickness, electrodeposition time of PANI and rotating rate on the current response of the composite modified electrode toward H2O2 were optimized to obtain the maximal sensitivity. A linear range from 8 × 10−9 to 5 × 10−6 M for H2O2 detection has been observed at the PB/PANI/MWNTs modified GCE with a correlation coefficient of 0.997. The detection limit is 5 × 10−9 M on signal-to-noise ratio of 3. To the best of our knowledge, this is the lowest detection limit for H2O2 detection. The electrode also shows high sensitivity (526.43 μA μM−1 cm−2) for H2O2 detection which is more than three orders of magnitude higher than the reported.  相似文献   

6.
Gold nanoparticles (Au nps) have been synthesized in aqueous solution of polyvinyl pyrrolidone (PVP) by gamma radiolysis from HAuCl4·3H2O precursor and in presence of small concentrations of Ag+, 2-propanol and acetone. The effect of different experimental parameters, such as concentration of reactant, molecular weight of PVP on nanoparticle formation was studied. TEM image confirmed that spherical Au nps were formed when PVP of molecular weight 360,000 Da was used as capping agent. H2O2 is a reactant in the enzyme catalyzed reaction of o-phenylene diamine (o-PDA). The reaction product has a weak absorption in the yellow region of the spectrum. When this product interacts with Au nps, it leads to enhancement of the absorption peak. The nanoparticles synthesized by radiation method were used for estimation of H2O2. The absorbance value of this peak at λmax was observed to change with H2O2 concentration, which was monitored for estimation of H2O2. The response is linear in the range of 2.5×10−6 mol dm−3 to 2×10−4 mol dm−3 and 1×10−7 mol dm−3 to 3×10−6 mol dm−3 H2O2 in two separate sets of experimental parameters with detection limit 1×10−7 mol dm−3.  相似文献   

7.
Hua MY  Chen HC  Tsai RY  Lai CS 《Talanta》2011,85(1):631-637
The imine of polybenzimidazole (PBI) is chemically oxidized by hydrogen peroxide (H2O2) in the presence of acetic acid (AcOH). Fourier transform infrared (FT-IR) and X-ray photoelectron spectroscopies (XPS) showed that when the AcOH concentration remained constant, the degree of oxidation increased with increasing H2O2 levels. Moreover, the imine also exhibited electrochemical redox behavior. Based on these properties, a PBI-modified Au (PBI/Au) electrode was developed as an enzyme-free H2O2 sensor. At an applied potential of −0.5 V vs. Ag/AgCl, the current response of the PBI/Au electrode was linear with H2O2 concentration over a range from 0.075 to 1.5 mM, with a sensitivity of 55.0 μA mM−1 cm−2. The probe had excellent stability, with <5% variation from its initial response current after storage at 50 °C for 10 days. Potentially interfering species such as ascorbic or uric acid had no effect on sensitivity. Sensitivity improved dramatically when multiwalled carbon nanotubes (MWCNT) were incorporated in the probe. Under optimal conditions, the detection of H2O2 using a MWCNT-PBI/Au electrode was linear from 1.56 μM to 2.5 mM, with a sensitivity of 928.6 μA mM−1 cm−2. Analysis of H2O2 concentrations in urine samples using a MWCNT-PBI/Au electrode produced accurate real-time results comparable to those of traditional HPLC methods.  相似文献   

8.
A sandwich-type electrochemical immunosensor for the detection of carbohydrate antigen 19-9 (CA 19-9) antigen based on the immobilization of primary antibody (Ab1) on three dimensional ordered macroporous magnetic (3DOMM) electrode, and the direct electrochemistry of horseradish peroxidase (HRP) that was used as both the label of secondary antibody (Ab2) and the blocking reagent. The 3DOMM electrode was fabricated by introducing core–shell Au–SiO2@Fe3O4 nanospheres onto the surface of three dimensional ordered macroporous (3DOM) Au electrode via the application of an external magnet. Au nanoparticles functionalized SBA-15 (Au@SBA-15) was conjugated to the HRP labeled secondary antibody (HRP-Ab2) through the Au–SH or Au–NH3+ interaction, and HRP was also used as the block reagent. The formation of antigen–antibody complex made the combination of Au@SBA-15 and 3DOMM exhibit remarkable synergistic effects for accelerating direct electron transfer (DET) between HRP and the electrode. Under the optimal conditions, the DET current signal increased proportionally to CA 19-9 concentration in the range of 0.05 to 15.65 U mL−1 with a detection limit of 0.01 U mL−1. Moreover, the immunosensor showed high selectivity, good stability, satisfactory reproducibility and regeneration. Importantly, the developed method was used to assay clinical serum specimens, achieving a good relation with those obtained from the commercialized electrochemiluminescent method.  相似文献   

9.
A novel cobalt-tetraphenylporphyrin/reduced graphene oxide (CoTPP/RGO) nanocomposite was prepared by a π–π stacking interaction and characterized by ultraviolet–visible absorption spectroscopy (UV–vis), Fourier transform infrared spectroscopy (FTIR) and electrochemical impedance spectroscopy (EIS). The CoTPP/RGO nanocomposite exhibited high electrocatalytic activity both for oxidation and reduction of H2O2. The current response was linear to H2O2 concentration with the concentration range from 1.0 × 10−7 to 2.4 × 10−3 mol L−1 (R = 0.998) at the reductive potential of −0.20 V and from 1.0 × 10−7 to 4.6 × 10−4 mol L−1 (R = 0.996) at the oxidative potential of +0.50 V. The H2O2 biosensor showed good anti-interfering ability towards oxidative interferences at the oxidative potential of +0.50 V and good anti-interfering ability towards reductive interferences at the reductive potential of −0.20 V.  相似文献   

10.
Some nanostructures are reported to possess enzyme-mimetic activities similar to those of natural enzymes. Herein, highly-dispersed Pt nanodots on Au nanorods (HD- PtNDs@AuNRs) with mimetic peroxidase activity were designed as an active electrode modifier for fabrication of a hydrogen peroxide (H2O2) electrochemical sensor. The HD-PtNDs@AuNRs were synthesized by a seed-mediated growth approach and confirmed by scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray spectroscopy, and UV–vis spectroscopy. The electrochemical and catalytical performances of HD-PtNDs@AuNRs towards H2O2 reduction were investigated in detail by cyclic voltammetry and amperometry. The HD-PtNDs@AuNRs modified electrode displayed a high catalytic activity to H2O2 at −0.10 V (versus SCE), a rapid response within 5 s, a wide linear range of 2.0–3800.0 μM, a detection limit of 1.2 μM (S/N = 3), and a high sensitivity of 181 μA mM−1 cm−2. These results suggested a promising potential of fabricating H2O2 electrochemical sensor using HD- PtNDs@AuNRs.  相似文献   

11.
Recent progress in flexible and lightweight electrochemical sensor systems requires the development of paper-like electrode materials. Here, we report a facile and green synthesis of a new type of MnO2 nanowires–graphene nanohybrid paper by one-step electrochemical method. This strategy demonstrates a collection of unique features including the effective electrochemical reduction of graphene oxide (GO) paper and the high loading of MnO2 nanowires on electrochemical reduced GO (ERGO) paper. When used as flexible electrode for nonenzymatic detection of hydrogen peroxide (H2O2), MnO2–ERGO paper exhibits high electrocatalytic activity toward the redox of H2O2 as well as excellent stability, selectivity and reproducibility. The amperometric responses are linearly proportional to H2O2 concentration in the range 0.1–45.4 mM, with a detection limit of 10 μM (S/N = 3) and detection sensitivity of 59.0 μA cm−2 mM−1. These outstanding sensing performances enable the practical application of MnO2–ERGO paper electrode for the real-time tracking H2O2 secretion by live cells macrophages. Therefore, the proposed graphene-based nanohybrid paper electrode with intrinsic flexibility, tailorable shapes and adjustable properties can contribute to the full realization of high-performance flexible electrode material used in point-of-care testing devices and portable instruments for in-vivo clinical diagnostics and on-site environmental monitoring.  相似文献   

12.
A novel nonenzymatic sandwich-type electrochemical immunosensor has been developed to detect squamous cell carcinoma antigen (SCCA). Nitrogen-doped graphene sheet (N-GS) was used to increase capacity of capturing primary antibodies (Ab1). Carbon-supported Pd–Au binary nanoparticles (Pd–Au/C) were synthesized and used to label secondary antibodies (Ab2). The specific binding of SCCA and antibodies enabled a quantitative attachment of Pd–Au/C on the electrode surface. Electrocatalytic analysis showed that the prepared Pd–Au/C exhibit excellent electrocatalytic activity towards hydrogen peroxide (H2O2). We use current response of electrocatalytic labels Pd–Au/C to detect the concentration of SCCA. The unique nonenzymatic immunosensor exhibits a relatively wide linear range from 0.005 to 2 ng mL−1 and high sensitivity with a low detection limit of 1.7 pg mL−1. The immunsensor also shows good reproducibility (4.2%) and stability (5.8%), which makes it an enormous application prospect in clinical research.  相似文献   

13.
In this study, we developed a fluorescence assay for the highly sensitive and selective detection of Hg2+ and Pb2+ ions using a gold nanoparticle (Au NP)-based probe. The Hg–Au and Pb–Au alloys that formed on the Au NP surfaces allowed the Au NPs to exhibit peroxidase-mimicking catalytic activity in the H2O2-mediated oxidation of Amplex UltraRed (AUR). The fluorescence of the AUR oxidation product increased upon increasing the concentration of either Hg2+ or Pb2+ ions. By controlling the pH values of 5 mM tris–acetate buffers at 7.0 and 9.0, this H2O2–AUR–Au NP probe detected Hg2+ and Pb2+ ions, respectively, both with limits of detection (signal-to-noise ratio: 3) of 4.0 nM. The fluorescence intensity of the AUR oxidation product was proportional to the concentrations of Hg2+ and Pb2+ ions over ranges 0.05–1 μM (R2 = 0.993) and 0.05–5 μM (R2 = 0.996), respectively. The H2O2–AUR–Au NP probe was highly selective for Hg2+ (>100-fold) and Pb2+ (>300-fold) ions in the presence of other tested metal ions. We validated the practicality of this simple, selective, and sensitive H2O2–AUR–Au NP probe through determination of the concentrations of Hg2+ and Pb2+ ions in a lake water sample and of Pb2+ ions in a blood sample. To the best of our knowledge, this system is the first example of Au NPs being used as enzyme-mimics for the fluorescence detection of Hg2+ and Pb2+ ions.  相似文献   

14.
JingJing Xu  Yuan Tian  Litong Jin 《Talanta》2010,82(4):1511-1515
A highly soluble poly(3,4-ethylenedioxythiophene)-poly(styrene sulfonic acid)/Au (PEDOT-PSS/Au) nanocomposite was prepared via one-step chemical synthesis and the matrix was characterized by UV-vis spectroscopy (UV-vis), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM) and transmission electron microscope (TEM). Due to the excellent aqueous compatibility and biocompatibility, the PEDOT/PSS-Au nanocomposite can be used as biomaterial for enzymes immobilization. In this system, redox enzyme, horseradish peroxidase (HRP) was integrated with PEDOT/PSS-Au nanocomposite and the direct electron transfer of HRP was observed. Moreover, we find that the HRP/PEDOT-PSS/Au modified electrode shows excellent electrocatalytic ability for H2O2 and the formal Michaelis-Menten constant was 0.78 mmol/L. The response currents have good linear relation with the concentrations of H2O2 with a linear range from 2.0 × 10−7 to 3.8 × 10−4 mol/L.  相似文献   

15.
A colloidal suspension of nanostructured poly(N-butyl benzimidazole)-graphene sheets (PBBIns-Gs) was used to modify a gold electrode to form a three-dimensional PBBIns-Gs/Au electrode that was sensitive to hydrogen peroxide (H2O2) in the presence of acetic acid (AcOH). The positively charged nanostructured poly(N-butyl benzimidazole) (PBBIns) separated the graphene sheets (Gs) and kept them suspended in an aqueous solution. Additionally, graphene sheets (Gs) formed “diaphragms” that intercalated Gs, which separated PBBIns to prevent tight packing and enhanced the surface area. The PBBIns-Gs/Au electrode exhibited superior sensitivity toward H2O2 relative to the PBBIns-modified Au (PBBIns/Au) electrode. Furthermore, a high yield of glucose oxidase (GOD) on the PBBIns-Gs of 52.3 mg GOD per 1 mg PBBIns-Gs was obtained from the electrostatic attraction between the positively charged PBBIns-Gs and negatively charged GOD. The non-destructive immobilization of GOD on the surface of the PBBIns-Gs (GOD-PBBIns-Gs) retained 91.5% and 39.2% of bioactivity, respectively, relative to free GOD for the colloidal suspension of the GOD-PBBIns-Gs and its modified Au (GOD-PBBIns-Gs/Au) electrode. Based on advantages including a negative working potential, high sensitivity toward H2O2, and non-destructive immobilization, the proposed glucose biosensor based on an GOD-PBBIns-Gs/Au electrode exhibited a fast response time (5.6 s), broad detection range (10 μM to 10 mM), high sensitivity (143.5 μA mM−1 cm−2) and selectivity, and excellent stability. Finally, a choline biosensor was developed by dipping a PBBIns-Gs/Au electrode into a choline oxidase (ChOx) solution for enzyme loading. The choline biosensor had a linear range of 0.1 μM to 0.83 mM, sensitivity of 494.9 μA mM−1 cm−2, and detection limit of 0.02 μM. The results of glucose and choline measurement indicate that the PBBIns-Gs/Au electrode provides a useful platform for the development of oxidase-based biosensors.  相似文献   

16.
In this paper, LaNi0.6Co0.4O3 (LNC) nanoparticles were synthesized by the sol–gel method, and the structure and morphology of LNC nanoparticles were characterized by X-ray diffraction spectrum, scanning electron microscopy and transmitting electron microscopy. And then, LNC was used to modify carbon paste electrode (CPE) without any adhesive to fabricate hydrogen peroxide and glucose sensor, and the results demonstrated that LNC exhibited strong electrocatalytical activity by cyclic voltammetry and amperometry. In H2O2 determination, linear response was obtained in the concentration range of 10 nM–100 μM with a detection limit of 1.0 nM. In glucose determination, there was the linear region of 0.05–200 μM with a detection limit of 8.0 nM. Compared with other reports, the proposed sensor also displayed high sensitivity toward H2O2 (1812.84 μA mM−1 cm−2) and glucose (643.0 μA mM−1 cm−2). Moreover, this prepared sensor was applied to detect glucose in blood serum and hydrogen peroxide in toothpaste samples with satisfied results, indicating its possibility in practical application.  相似文献   

17.
In this work, we utilized polyethyleneimine-capped silver nanoclusters (PEI-Ag nanoclusters) to develop a new fluorometric method for the determination of hydrogen peroxide and glucose with high sensitivity. The PEI-Ag nanoclusters have an average size of 2 nm and show a blue emission at 455 nm. The photostable properties of the PEI-Ag nanoclusters were examined. The fluorescence of the PEI-Ag nanoclusters could be particularly quenched by H2O2. The oxidization of glucose by glucose oxidase coupled with the fluorescence quenching of PEI-Ag nanoclusters by H2O2 can be used to detect glucose. Under optimum conditions, the fluorescence intensity quenched linearly in the range of 500 nM–100 μM with high sensitivity. The detection limit for H2O2 was 400 nM. And a linear correlation was established between fluorescence intensity (F0 − F) and concentration of glucose in the range of 1.0 × 10−6 to 1.0 × 10−5 M and 1.0 × 10−5 to 1.0 × 10−3 M with a detection limit of 8.0 × 10−7 M. The method was used for the detection of glucose in human serum samples with satisfactory results. Furthermore, the mechanism of sensitive fluorescence quenching response of Ag nanoclusters to glucose and H2O2 has been discussed.  相似文献   

18.
The aluminium(III)–citrate complex (NH4)4[Al2(C6H4O7)(C6H5O7)2]·4H2O was characterized using anion exchange chromatography on-line coupled with the element specific ICP-AES detector. Time-dependent monitoring of individual species in aqueous solution at different temperatures gave information about the species stability and the decomposition pathway. The aluminium–citrate complex (NH4)4[Al2(C6H4O7)(C6H5O7)2]·4H2O disintegrated via an unknown intermediary Al(III)–citrate species from which the thermodynamically stable complex [Al3(C6H4O7)3(OH)(H2O)]4− was formed. The activation energy for the decomposition reaction and the pre-exponential factor were determinated to be Ea = 81.95 kJ mol−1 and A = 3.62 × 1013 s−1.  相似文献   

19.
Phosphomolybdate, H3PMo12O40, (PMo12)-doped-poly(3,4-ethylenedioxythiophene) (PEDOT) coated gold nanoparticles have been synthesized in aqueous solution by reduction of AuCl4 using hydroxymethyl EDOT as a reducing agent in the presence of polystyrene sulfonate and PMo12. The resulting PMo12-doped-PEDOT stabilized Au nanoparticles are water soluble and have been characterized by UV–visible spectroscopy, scanning electron microscopy and electrochemistry. Glassy carbon electrodes modified with these Au nanoparticles show excellent stability and catalytic activity towards the reduction of bromate in an aqueous electrolyte solution containing 10 mM H2SO4 and 0.1 M Na2SO4.  相似文献   

20.
Xiujie Bian  E. Jin 《Talanta》2010,81(3):813-83
Pt/polypyrrole (PPy) hybrid hollow microspheres were successfully prepared by wet chemical method via Fe3O4 template and evaluated as electrocatalysts for the reduction of hydrogen peroxide. The as-synthesized products were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectra (XPS), X-ray diffraction (XRD), inductive coupled plasma emission spectrum (ICP) and Fourier-transform infrared spectra (FTIR) measurements. The results exhibited that ultra-high-density Pt nanoparticles (NPs) were well deposited on the PPy shell with the mean diameters of around 4.1 nm. Cyclic voltammetry (CV) results demonstrated that Pt/PPy hybrid hollow microspheres, as enzyme-less catalysts, exhibited good electrocatalytic activity towards the reduction of hydrogen peroxide in 0.1 M phosphate buffer solution (pH = 7.0). The composite had a fast response of less than 2 s with linear range of 1.0-8.0 mM and a relatively low detection limit of 1.2 μM (S/N = 3). The sensitivity of the sensor for H2O2 was 80.4 mA M−1 cm−2.  相似文献   

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