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1.
Sensitive fluorescent probes for the determination of hydrogen peroxide and glucose were developed by immobilizing enzyme horseradish peroxidase (HRP) on Fe3O4/SiO2 magnetic core–shell nanoparticles in the presence of glutaraldehyde. Besides its excellent catalytic activity, the immobilized enzyme could be easily and completely recovered by a magnetic separation, and the recovered HRP-immobilized Fe3O4/SiO2 nanoparticles were able to be used repeatedly as catalysts without deactivation. The HRP-immobilized nanoparticles were able to activate hydrogen peroxide (H2O2), which oxidized non-fluorescent 3-(4-hydroxyphenyl)propionic acid to a fluorescent product with an emission maximum at 409 nm. Under optimized conditions, a linear calibration curve was obtained over the H2O2 concentrations ranging from 5.0 × 10−9 to 1.0 × 10−5 mol L−1, with a detection limit of 2.1 × 10−9 mol L−1. By simultaneously using glucose oxidase and HRP-immobilized Fe3O4/SiO2 nanoparticles, a sensitive and selective analytical method for the glucose detection was established. The fluorescence intensity of the product responded well linearly to glucose concentration in the range from 5.0 × 10−8 to 5.0 × 10−5 mol L−1 with a detection limit of 1.8 × 10−8 mol L−1. The proposed method was successfully applied for the determination of glucose in human serum sample.  相似文献   

2.
The electrode characteristics and selectivities of PVC-based thiocyanate selective polymeric membrane electrode (PME) incorporating the newly synthesized zinc complex of 6,7:14,15-Bzo2-10,11-(4-methylbenzene)-[15]-6,8,12,14-tetraene-9,12-N2-1,5-O2 (I 1 ) and zinc complex of 6,7:14,15-Bzo2-10,11-(4-methylbenzene)-[15]-6,14-diene-9,12-dimethylacrylate-9,12-N2-1,5-O2 (I 2 ) are reported here. The best response was observed with the membrane having a composition of I2:PVC:o-NPOE:HTAB in the ratio of 6:33:59:2 (w/w; milligram). This electrode exhibited Nernstian slope for thiocyanate ions over working concentration range of 4.4 × 10−7 to 1.0 × 10−2 mol L−1 with detection limit of 2.2 × 10−7 mol L−1. The performance of this electrode was compared with coated graphite electrode (CGE), which showed better response characteristics w.r.t Nernstian slope 59.0 ± 0.2 mV decade−1 activity, wide concentration range of 8.9 × 10−8 to 1.0 × 10−2 mol L−1 and detection limit of 6.7 × 10−8 mol L−1. The response time for CGE and PME was found to be 8 and 10 s, respectively. The proposed electrode (CGE) was successfully applied to direct determination of thiocyanate in biological and environmental samples and also as indicator electrode in potentiometric titration of SCN ion.  相似文献   

3.
N,N-dimethylhydroxylamine (DMHA) is a novel salt-free reducing reagent used in the separation U from Pu and Np in the reprocessing of power spent fuel. This paper reports on the radiolysis of aqueous DMHA solution and its radiolytic liquid organics. Results show that the main organics in irradiated DMHA solution are N-methyl hydroxylamine, formaldehyde and formic acid. The analysis of DMHA and N-methyl hydroxylamine were performed by gas chromatography, and that of formaldehyde was performed by ultraviolet–visible spectrophotometry. The analysis of formic acid was performed by ion chromatography. For 0.1–0.5 mol L−1 DMHA irradiated to 5–25 kGy, the residual DMHA concentration is (0.07–0.47) mol L−1, the degradation rate of DMHA at 25 kGy is 10.1–30.1%. The concentrations of N-methylhydroxylamine, formaldehyde and formic acid are (8.25–19.36) × 10−3, (4.20–36.36) × 10−3 and (1.35–10.9) × 10−4 mol L−1, respectively. The residual DMHA concentration decreases with the increasing dose. The concentrations of N-methylhydroxylamine and formaldehyde increase with the dose and initial DMHA concentration, and that of formic acid increases with the dose, but the relationship between the concentration of formic acid and initial DMHA concentration is not obvious.  相似文献   

4.
Thermally two-dimensional lattice graphene (GR) and biocompatibility chitosan (CS) act as a suitable support for the deposition of palladium nanoparticles (PdNPs). A novel hydrogen peroxide (H2O2) biosensor based on immobilization of hemoglobin (Hb) in thin film of CS containing GR and PdNPs was developed. The surface morphologies of a set of representative membranes were characterized by means of scanning electron microscopy and showed that the PdNPs are of a sphere shape and an average diameter of 50 nm. Under the optimal conditions, the immobilized Hb showed fast and excellent electrocatalytic activity to H2O2 with a small Michaelis–Menten constant of 16 μmol L−1, a linear range from 2.0 × 10−6 to 1.1 × 10−3 mol L−1, and a detection limit of 6.6 × 10−7 mol L−1. The biosensor also exhibited other advantages, good reproducibility, and long-term stability, and PdNPs/GR–CS nanocomposites film would be a promising material in the preparation of third generation biosensor.  相似文献   

5.
A simple sensor based on bare carbon ionic liquid electrode was fabricated for simultaneous determination of dihydroxybenzene isomers in 0.1 mol L−1 phosphate buffer solution (pH 6.0). The oxidation peak potential of hydroquinone was about 0.136 V, catechol was about 0.240 V, and resorcinol 0.632 V by differential pulse voltammetric measurements, which indicated that the dihydroxybenzene isomers could be separated absolutely. The sensor showed wide linear behaviors in the range of 5.0 × 10−7–2.0 × 10−4 mol L−1 for hydroquinone and catechol, 3.5 × 10−6–1.535 × 10−4 mol L−1 for resorcinol, respectively. And the detection limits of the three dihydroxybenzene isomers were 5.0 × 10−8, 2.0 × 10−7, 5.0 × 10−7 mol L−1, respectively (S/N = 3). The proposed method could be applied to the determination of dihydroxybenzene isomers in artificial wastewater and the recovery was from 93.9% to 104.6%.  相似文献   

6.
In the present work, a new voltammetric sensor, Langmuir–Blodgett (LB) film of tetraoxocalix[2]arene[2]triazine (TOCT) modified glassy carbon electrode (LBTOCT-GCE), for trace analysis of copper ion in water samples, was prepared. The morphology of LBTOCT-GCE was characterized by cyclic voltammetric method, electrochemical impedance spectroscopy, and atomic force microscope. The recognizing mechanism of LBTOCT-GCE for copper ion in aqueous solution was discussed. Under the optimum experimental conditions, using square wave stripping voltammetry and accumulation time of 300 s, the peak currents were linear relationship with Cu2+ concentrations in the range of 2 × 10−9 to 1 × 10−6 mol L−1, with detection limit of 1 × 10−10 mol L−1. By this method, real samples (lake water, drinking water, and city wastewater) were analyzed with satisfactory results. In addition, the fabricated electrode exhibited a distinct advantage of simple preparation, non-toxicity, good reproducibility, and stability.  相似文献   

7.
A new H2O2 biosensor was fabricated on the basis of nanocomposite films of hemoglobin (Hb), silver nanoparticles (AgNPs), and multiwalled carbon nanotubes (MWNTs)–chitosan (Chit) dispersed solution immobilized on glassy carbon electrode (GCE). The immobilized Hb displayed a pair of well-defined and reversible redox peaks with a formal potential (E θ′) of −22.5 mV in 0.1 M pH 7.0 phosphate buffer solution. The apparent heterogeneous electron transfer rate constants (k s) in the Chit–MWNTs film was evaluated as 2.58 s−1 according to Laviron’s equation. The surface concentration (Γ*) of the electroactive Hb in the Chit–MWNTs film was estimated to be (2.48 ± 0.25) × 10−9 mol cm−2. Meanwhile, the Chit–MWNTs/Hb/AgNPs/GCE demonstrated excellently electrocatalytical ability to H2O2. Its apparent Michaelis–Menten constant (K Mapp) for H2O2 was 0.0032 mM, showing a good affinity. Under optimal conditions, the biosensors could be used for the determination of H2O2 ranging from 6.25 × 10−6 to 9.30 × 10−5 mol L−1 with a detection limit of 3.47 × 10−7 mol L−1 (S/N = 3). Furthermore, the biosensor possessed rapid response to H2O2 and good stability, selectivity, and reproducibility.  相似文献   

8.
Simple and sensitive electrochemical method for the determination of nitrite, based on a nano-alumina-modified glassy carbon electrode (GCE), is described. Nitrite yields a well-defined oxidation peak whose potential is 0.74 V at the nano-alumina-coated GCE in 0.1 mol L−1 phosphate buffer (pH 5.0). Compared with bare GCE, the nano-alumina-modified GCE has evident catalytic effect towards the oxidation of nitrite, and its peak current can be significantly enhanced. Some of the experimental parameters were optimized for the determination of nitrite. The oxidation peak current was proportional to nitrite concentration in the range of 5.0 × 10−8–1.1 × 10−3 mol L−1, and a detection limit of 1.0 × 10−8 mol L−1 was obtained. This method has been successfully used to the determination of nitrite in sausage sample. Furthermore, results obtained by the method have been compared with spectrophotometric method.  相似文献   

9.

Abstract  

This article proposes a simple and fast method of In(III) determination in the presence of Cd(II) and Pb(II). The catalytic activity of N-methylthiourea was used in the In(III) electroreduction, which also had a slight effect on the electroreduction process of Cd(II) and Pb(II). By applying square wave voltammetry it was possible to determine 3 × 10−7 mol dm−3 In(III) in the presence of 5 × 10−5 mol dm−3 Cd(II) and 1 × 10−4 mol dm−3 Pb(II) in 5 mol dm−3 NaClO4 at pH 2. The calibration curve for In(III) was linear from 3 × 10−7 to 5 × 10−4 mol dm−3. The relative standard deviation for In(III) determination was about 3.0%.  相似文献   

10.
A new adsorbent is proposed for the solid-phase extraction of phenol and 1-naphthol from polluted water. The adsorbent (TX-SiO2) is an organosilica composite made from a bifunctional immobilized layer comprising a major fraction (91%) of hydrophilic diol groups and minor fraction (9%) of the amphiphilic long-chain nonionic surfactant Triton X-100 (polyoxyethylated isooctylphenol) (TX). Under static conditions phenol was quantitatively extracted onto TX-SiO2 in the form of a 4-nitrophenylazophenolate ion associate with cetyltrimethylammonium bromide. The capacity of TX-SiO2 for phenol is 2.4 mg g−1 with distribution coefficients up to 3.4 × 104 mL g−1; corresponding data for 1-naphthol are 1.5 mg g−1 and 3 × 103 mL g−1. The distribution coefficient does not change significantly for solution volumes of 0.025–0.5 L and adsorbent mass less than 0.03 g; 1–90 μg analyte can be easily eluted by 1–3 mL acetonitrile with an overall recovery of 98.2% and 78.3% for phenol and 1-naphthol, respectively. Linear correlation between acetonitrile solution absorbance (A 540) and phenol concentration (C) in water was found according to the equation A 540 = (6 ± 1) × 10−2 + (0.9 ± 0.1)C (μmol L−1) with a detection range from 1 × 10−8 mol L−1 (0.9 μL g−1) to 2 × 10−7 mol L−1 (19 μL g−1), a limit of quantification of 1 μL g−1 (preconcentration factor 125), correlation coefficient of 0.936, and relative standard deviation of 2.5%. A solid-phase colorimetric method was developed for quantitative determination of 1-naphthol on adsorbent phase using scanner technology and RGB numerical analysis. The detection limit of 1-naphthol with this method is 6 μL g−1 while the quantification limit is 20 μL g−1. A test system was developed for naked eye monitoring of 1-naphthol impurities in water. The proposed test kit allows one to observe changes in the adsorbent color when 1-naphthol concentration in water is 0.08–3.2 mL g−1.  相似文献   

11.
The electrooxidative behaviour and determination of quetiapine (QTP), a dibenzothiazepine derivative and antipsychotic agent, on a glassy carbon disc electrode was investigated using cyclic (CV), linear sweep (LSV), differential pulse (DPV) and Osteryoung square wave voltammetry (OSWV). Fully validated DP and SW voltammetric procedures are described for the determination of QTP. QTP in pH 3.5 acetate buffer solution presents a well-defined anodic response, studied by the proposed methods. This main response was due to the irreversible, diffusion-controlled, one-electron and one-proton oxidation of the aliphatic nitrogen of the piperazine ring. Under optimal conditions, a detection limit of 4.0 × 10−8 mol L−1 for DPV and 1.33 × 10−7 mol L−1 for OSWV, and a linear calibration graph in the range from 4.0 × 10−6 to 2.0 × 10−4 mol L−1 were obtained for both methods. The procedure was successfully applied to the determination of the drug in tablets, human serum and human urine with good recoveries. The detection limits were 6.20 × 10−7 mol L−1 and 5.92 × 10−7 mol L−1 in human serum and 1.44 × 10−7 mol L−1 and 1.31 × 10−6 mol L−1 in human urine, for the DPV and OSWV method, respectively.  相似文献   

12.
A novel voltammetric sensor, based on single-walled carbon nanotubes (SWNT) dispersed in Nafion and modified glassy carbon electrode (GCE), was fabricated and used to determine the trace amounts of dihydromyricetin (DMY). The electrochemical behavior of DMY at this sensor was investigated in 0.1 mol L−1 sulfuric acid solutions + 0.1 mol L−1 NaCl by cyclic voltammetry and squarewave voltammetry. Compared with bare GCE, the electrode presented an excellent response of DMY through an adsorption-controlled quasi-reversible process. Under the optimum conditions, the response peak currents were linear relationship with the DMY concentrations in the range of 1.0 × 10−7–1.0 × 10−5 mol L−1 with a detection limit of 9 × 10−8 mol L−1. Based on this voltammetric sensor, a simple and sensitive electroanalytical method for DMY was proposed and applied to quantitative determination of DMY in Ampelopsis grossedentata samples. In addition, the oxidation mechanism was proposed and discussed, which could be a reference for the pharmacological action of DMY in clinical study.  相似文献   

13.
A Nafion/multi-wall carbon nanotubes (MWNT) composite film-modified electrode was fabricated. The modified electrode showed excellent electrocatalytic activity toward ascorbic acid (AA) and uric acid (UA) in 0.1-mol L−1 NaCl medium (pH 6.5). Compared to the bare electrode that only displayed a broad and overlapped oxidation peak, the Nafion/MWNT film-modified electrode not only remarkably enhanced the anodic peak currents of AA and UA but also avoided the overlapping of the anodic peaks of AA and UA with a 320-mV separation of both peaks. Under the optimized conditions, the peak currents of AA and UA were proportional to their concentration at the ranges of 8.0 × 10−5 to 6.0 × 10−3 mol L−1 and 6.0 × 10−7 to 8.0 × 10−5 mol L−1, respectively. The proposed method was used for the detection of AA and UA in real samples with satisfactory results.  相似文献   

14.
A multicommutation-based flow system with photometric detection was developed, employing an analytical microsystem constructed with low temperature co-fired ceramics (LTCC) technology, a solid-phase reactor containing particles of Canavalia ensiformis DC (urease source) immobilized with glutaraldehyde, and a mini-photometer coupled directly to the microsystem which monolithically integrates a continuous flow cell. The determination of urea in milk was based on the hydrolysis of urea in the solid-phase reactor and the ammonium ions produced were monitored using the Berthelot reaction. The analytical curve was linear in the urea concentration range from 1.0 × 10−4 to 5.0 × 10−3 mol L−1 with a limit of detection of 8.0 × 10−6 mol L−1. The relative standard deviation (RSD) for a 2.0 × 10−3 mol L−1 urea solution was lower than 0.4% (n = 10) and the sample throughput was 13 h−1. To check the reproducibility of the flow system, calibration curves were obtained with freshly prepared solutions on different days and the RSD obtained was 4.7% (n = 6). Accuracy was assessed by comparing the results of the proposed method with those from the official procedure and the data are in close agreement, at a 95% confidence level.  相似文献   

15.
A sensitive molecularly imprinted electrochemical sensor was developed for selective detection of streptomycin by combination of mercaptoacetic acid-modified PbS nanoparticles with Au-coated Fe3O4 magnetic nanoparticles dispersed multi-walled carbon nanotubes doped chitosan film. The imprinted sensor was fabricated onto the Au electrode via stepwise modification of nanocomposites and an electrodeposited thin film of molecularly imprinted polymers via sol–gel technology. The morphologies and electrochemical behaviors of the imprinted sensor were characterized by scanning electron microscope, cyclic voltammetry, and differential pulse voltammetry, respectively. The prepared sensor showed very high recognition ability and selectivity for streptomycin. Under optimal conditions, the imprinted sensor displayed good electrocatalytic activity to the redox of streptomycin. And the differential voltammetric anodic peak current was linear to the logarithm of streptomycin concentration in the range from 1.0 × 10−6 to 1.0 × 10−3 mol L−1, and the detection limit obtained was 1.5 × 10−9 mol L−1. This proposed imprinted sensor was used successfully for streptomycin determination in different injection solution samples.  相似文献   

16.
The corrosion inhibition of X-70 pipeline steel in saltwater saturated with CO2 at 50 °C with carboxyamido imidazoline has been evaluated by using electrochemical techniques. Techniques included polarization curves, linear polarization resistance, electrochemical impedance, and electrochemical noise measurements. Inhibitor concentrations were 0, 1.6 × 10−5, 3.32 × 10−5, 8.1 × 10−5, 1.6 × 10−4, and 3.32 × 10−4 mol l−1. All techniques showed that the best corrosion inhibition was obtained by adding 8.1 × 10−5 mol l−1 of carboxyamido imidazoline. For inhibitor concentrations higher than 8.1 × 10−5 mol l−1 a desorption process occurs, and an explanation has been given for this phenomenon.  相似文献   

17.
Electrochemical DNA biosensor was successfully developed by depositing the ionic liquid (e.g., 1-ethyl-3-methylimidazolium trifluoromethanesulfonate ([EMIM][Otf])), ZnO nanoparticles, and chitosan (CHIT) nanocomposite membrane on a modified gold electrode (AuE). The electrochemical properties of the [EMIM][Otf]/ZnO/CHIT/AuE for detection of DNA hybridization were studied. Under optimal conditions using cyclic voltammetry, the target DNA sequences could be detected in the concentration range of 1.0 × 10−18 to 1.82 × 10−4 mol L−1, and with the detection limit of 1.0 × 10−19 mol L−1. This DNA biosensor detection approaches provide a quick, sensitive, and convenient method to be used in the identification of Trichoderma harzianum.  相似文献   

18.
The electrochemical behavior of epinephrine (EP) at a mercaptoacetic acid (MAA) self-assembled monolayer modified gold electrode was studied. The MAA/Au electrode is demonstrated to promote the electrochemical response of epinephrine by cyclic voltammetry. The possible reaction mechanism is also discussed. The diffusion coefficient D of EP is 6.85 × 10−6 cm2 s−1. In 0.1 mol L−1 phosphate buffer (pH 7.20), a sensitive oxidation peak was observed at 0.177 V, and the peak current is proportional to the concentration of EP in the range of 1.0 × 10−5–2.0 × 10−4 mol L−1 and 1.0 × 10−7–1.0 × 10−6 mol L−1. The detection limit is 5 × 10−8 mol L−1. The modified electrode is highly stable and can be applied to the determination of EP in practical injection samples. The method is simple, quick, sensitive and accurate.  相似文献   

19.
The protonation and deprotonation of the Nb2O5 surface has been followed in order to understand the reactions of surface of this catalyst. The simultaneous potentiometric and conductometric titrations had been carried by using 50 mL of water suspension of Nb2O5 40 g L−1. The oxide was entirely deprotonated when adding 0.4 mL NaOH 1 mol L−1, and later titrated with 0.1 mol L−1. The titration had supplied K 1 and K 2 and the obtained values were 3.24 × 10−3 and 4.17 × 10−8, respectively. The zero point charge was pHpcz = 4.94. The thermodynamic studies were carried out by using 50 mL of a 40 g/L Nb2O5 aqueous suspension with the pH adjusted to pHPZC value. The suspension was titrated with 0.5 mol/L of HNO3 or NaOH for protonation or deprotonation studies, respectively, in an isoperibol calorimeter CSC ISC-4300. Thus, the obtained thermodynamic values of the protonation and deprotonation of Nb2O5 were Δdp G = −37.60 kJ/mol, Δdp H = −23.72 kJ/mol and ΔdpS = 47 J/(mol K).  相似文献   

20.
A carbon past electrode modified with [Mn(H2O)(N3)(NO3)(pyterpy)], ( \textpyterpy = 4¢- ( 4 - \textpyridyl ) - 2,2¢:\text6¢,\text2¢¢- \textterpyridine ) \left( {{\text{pyterpy}} = 4\prime - \left( {4 - {\text{pyridyl}}} \right) - 2,2\prime:{\text{6}}\prime,{\text{2}}\prime\prime - {\text{terpyridine}}} \right) complex have been applied to the electrocatalytic oxidation of nitrite which reduced the overpotential by about 120 mV with obviously increasing the current response. Relative standard deviations for nitrite determination was less than 2.0%, and nitrite can be determined in the ranges of 5.00 × 10−6 to 1.55 × 10−2 mol L−1, with a detection limit of 8 × 10−7 mol L−1. The treatment of the voltammetric data showed that it is a pure diffusion-controlled reaction, which involves one electron in the rate-determining step. The rate constant k′, transfer coefficient α for the catalytic reaction, and diffusion coefficient of nitrite in the solution, D, were found to be 1.4 × 10−2, 0.56× 10−6, and 7.99 × 10−6 cm2 s−1, respectively. The mechanism for the interaction of nitrite with the Mn(II) complex modified carbon past electrode is proposed. This work provides a simple and easy approach to detection of nitrite ion. The modified electrode indicated reproducible behavior, anti-fouling properties, and stability during electrochemical experiments, making it particularly suitable for the analytical purposes.  相似文献   

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