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1.
A new and simple photoelectrochemical (PEC) sensor using a glassy carbon electrode (GCE) modified with bismuth vanadate (BiVO4) nanoparticles and dihexadecyl phosphate (DHP) film was useful for acetaminophen (AC) determination. In 0.2 mol L−1 phosphate buffer (pH=9), the GCE without modification exhibited the smaller photocurrent (0.86 μA) when compared with GCE modified with 1.0 mg mL−1 or 2.0 mg mL−1 BiVO4 nanoparticles suspension (5.9 and 34 μA, respectively). Based on the photocurrent signal generated through the interaction between GCE, BiVO4 and the energy of visible light a chronoamperometric method for AC determination was developed. The AC linear range concentration from 0.099 to 0.99 μmol L−1 and limits of detection and quantification of 0.027 and 0.091 μmol L−1, respectively, was obtained. The proposed method was applied to the AC determination in commercial drugs and tap water with satisfactory accuracy and precision. Moreover, the PEC construction was easy and had a short response time, which might confer higher sample throughput for the method.  相似文献   

2.
A simple field method which allows the determination of fluoride in drinking water with a small handheld instrument called Arsenator was developed. Arsenator is a commercially available instrument which was used successfully for reliable determination of arsenic. In the proposed method the functionality of the Arsenator which is based on a photometric measurement of a spot on the reagent paper is expanded to analyse fluoride. A polymeric aluminium complex of 5-(2-carboxyphenylazo)-8-hydroxyquinoline (LH2) has been prepared as a new specific reagent for fluoride. Job's method of continuous variation was adopted for the determination of the composition of the coloured complex, which was further characterized by UV-VIS spectroscopic studies. The molar absorptivity of the complex formation is 8.48?×?103?L?mol?1?cm?1 at 410?nm. The coloured complex reacts with fluoride on an impregnated paper where its colour changes are dependent on the concentration of fluoride in water samples. The change in the colour was measured using the Arsenator. The method allows a reliable determination of fluoride in the range 0.3 to 2.0?mg?L?1. Further spectophotometric determinations of fluoride in drinking water were also studied. The determination is based on the reaction of aluminium complex with fluoride in the examined samples. Beer's law is obeyed in the range 0.3 to 2.0?mg?L?1 of fluoride at 495?nm. Sensitivity, detection limit and quantitation limit of the method were found to be 0.251?±?0.007?µg?1?mL, 0.1?mg?L?1 and 0.3?mg?L?1, respectively. The optimum reaction conditions and other analytical conditions were evaluated. The effect of interfering ions on the determination is described. There is no interference by nitrate or chloride. Sulphate interfered only at high concentrations which are not expected in drinking water.  相似文献   

3.
《Electroanalysis》2017,29(12):2793-2802
In this work, SiO2/Nb2O5/ZnO prepared by the sol‐gel processing method was used as substrate base for immobilization of the protoporphyrin‐IX ion. Iron(III) ion was inserted into the porphyrin ring (SiNbZn‐PPFe). A simple square wave voltammetry method based on a composite sensor carbon paste electrode of this material,designed as EPC‐SiNbZn‐PPFe, was developed and validated successfully for the determination of L‐tryptophan (Trp). The optimum conditions were obtained by using sensor modified with 18.00 mg SiNbZn‐PPFe material, 12.00 mg graphite powder and 6.0 μL mineral oil and phosphate buffer 0.3 mol L−1 pH 7.0. The sensitivity of the sensor was found to be 0.523 AL mol −1, linear range from 10 to 70 μmol L−1 and limit of detection of 3.28 μmol L−1. Therefore, the developed method was successfully applied for the Trp determination in real samples of pharmaceutical formulation and can be used for routine quality control pharmaceutical formulations containing Trp.  相似文献   

4.
《Electroanalysis》2017,29(10):2316-2322
A home‐made gold microelectrode (Au‐μE) was fabricated and its surface was modified with nanoporous gold structures via a facile electrochemical approach (anodization followed by electrochemical reduction method). The fabricated nanoporous Au microelectrode (NPG‐μE) was used as a sensor probe for the determination of As(III) in 1.0 mol L−1 HCl solution using square wave anodic stripping voltammetry (SWASV) technique. Field emission scanning electron microscopy (FE‐SEM) and cyclic voltammetry were used to characterize the surface morphology and assess the electrochemical surface area and the roughness factor of the NPG‐μE. SWASVs recorded with the NPG‐μE in As(III) solutions indicated linear behaviour in the concentration ranges of 10–200 μg L−1 and 2–30 μg L−1, with regression coefficients of 0.996 and 0.999 at a deposition time of 120 s, respectively. The limit of detection (LOD) was found to be 0.62 μg L−1 with high sensitivity of 29.75 μA (μg L−1)−1 cm−2. Repeatability and reproducibility were also examined and values were determined as 3.2 % and 9.0 %. Negligible interference from major interfering copper ion was noticed, revealing the excellent anti‐interference property of the proposed sensing platform. The developed NPG‐μE was successfully used for As(III) determination in tap water samples.  相似文献   

5.
It is significant to develop a point-of-care testing (POCT) method for rapid detection of medicinal molecules. In this paper, a graphdiyne (GDY)-ionic liquid (IL) composite was prepared via one-step facile ultrasound preparation process and then modified on gold (Au) electrode surface by simple casting method. Scanning electron microscopy and transmission electron microscopy were used to characterize the morphology of GDY-IL composite. Cyclic voltammetric results proved that GDY-IL composite on the electrode surface could effectively improve electron transfer rate, which meant that GDY-IL composite had high conductivity with big surface area. Finally, the modified electrode exhibited excellent performances for rutin detection with wider linear range (8.0×10−9 mol L−1–2.0×10−6 mol L−1 and 2.0×10−6 mol L−1–1.5×10−4 mol L−1) and lower detection limit (2.7 nmol L−1, 3S0/S). The Nafion/GDY-IL/Au electrode showed good sensitivity and high selectivity, which was satisfactory in analytical application to real samples. Therefore, the GDY-IL composite modified electrode has the potential applications in the POCT for electrochemical analysis of various medicinal molecules.  相似文献   

6.
《Tetrahedron letters》2014,55(51):7094-7098
A new thiacalix[4]arene based fluorescent chemosensor thiacalix[4]arene-N-(quinolin-8-yl)acetamide (TCAN8QA) has been synthesized. TCAN8QA has been found to exhibit highly selective behavior for F ions among all other anions, that is, Cl, Br, I, PO4−3, OH, H2PO4, and CH3COO in the absorption spectra as well as in the emission spectra. Red shift and quenching in emission spectra constituting the signature for fluoride detection are due to photoinduced charge transfer (PCT) which can be attributed to deprotonation of acidic NH proton in the presence of fluoride ions.  相似文献   

7.
《Arabian Journal of Chemistry》2020,13(11):7970-7977
The World Health Organization (WHO) has recommended the fluoride level in drinking water (1.5 mg/L) and defluoridation of water is an essential to remove of fluoride from contaminated water. Hence, the effective and rapid adsorbent Cuprous oxide-reduced graphene oxide (Cu2O-RGO) composite was developed to overwhelm this concern. Sonochemical approach was adopted for the synthesis of desirable composite which was further characterized by XRD, FTIR, SEM, and EDS. The optimized composite (30 mg) shown the significant adsorption capacity of 34 mg/g of F solution (pH = 9), 70% removal of F solution from real experiment and Freundlich model was fitted than Langmuir and Temkin isotherms. The experimental results corroborate that adsorbent is the most effective for removal of fluoride from its polluted water.  相似文献   

8.
《Electroanalysis》2017,29(12):2698-2707
A cholesterol biosensor based on cholesterol oxidase‐poly(diallyldimethylammonium chloride)‐carbon nanotubes‐nickel ferrite nanoparticles (ChOx‐PDDA‐CNTs‐NiFe2O4NPs) solution is easily fabricated by using a single dropping step on a glassy carbon electrode (GCE) surface. This technique is an alternative way to reduce complexity, cost and time to produce the biosensor. The uniformly dispersed materials on the electrode surface enhance the catalytic reaction of cholesterol oxidase and electron transfer from the oxidation of hydrogen peroxide in the system. The nickel ferrite nanoparticles were synthesized by co‐precipitation and calcination at various temperatures. These nanoparticles were then characterized using field emission scanning electron microscopy (FE‐SEM), energy‐dispersive X‐ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FTIR), cyclic voltammetry (CV) and X‐ray diffraction (XRD). The synthesized material calcined at 700 °C was well defined and presented the octahedral metal stretching with cubic NiFe2O4NPs phase. In cyclic voltammetric study, the ChOx‐PDDA‐CNTs‐NiFe2O4NPs/GCE showed 0.43 s−1 charge transfer rate constant (K s), 7.79×10−6 cm2 s−1 diffusion coefficient value (D ), 0.13 mm2 electroactive surface area (A e) and 3.58×10−8 mol cm−2 surface concentration ( ). This modified electrode exhibits stability in term of percent relative standard deviation (%RSD=0.62 %, n=10), reproducibility (%RSD=0.81, n=10), high sensitivity (25.76 nA per mg L−1 cm−2), linearity from 1 to 5,000 mg L−1 (R2=0.998) with a low detection limit (0.50 mg L−1). Its Michaelis‐Menten constant (K m) was 0.14 mM with 0.92 μA maximum current (I max) and demonstrated good selectivity without the effects of electroactive species such as ascorbic acid, glucose and uric acid. The cholesterol biosensor was successfully applied to determine cholesterol levels in human blood samples, showing promise due to its simplicity and availability.  相似文献   

9.
In this report, we have shown that the encapsulation of the terbium 2-methylimidazole-4,5-dicarboxylic acid complex into inorganic host tetraethoxysilance is considered to be an efficient way for the design of anion sensors. Strong green emission still can be observed when it disperses in pure water. It was found that the luminescence of hybrid material was selectively turned off rapidly (1 s) by hydrogen sulfate compared with the addition of different anions such as F, Cl, Br and I. Thin film was successfully prepared and also could be a promising tool for recognizing HSO4.  相似文献   

10.
Contamination of natural water by mercury (Hg2+) and bismuth (Bi3+) metal ions have been extensively studied due to their toxic effects. A validated square-wave anodic stripping voltammetry (SW-ASV) method for determining Bi3+ and Hg2+ ions individually and simultaneously is described. A new electrochemical sensor was constructed using a gold (Au) electrode that has been modified with poly(1,2-diaminoanthraquinone) (p-1,2-DAAQ). Scanning electron microscopy, cyclic voltammetry, and electrochemical impedance spectroscopy were used to characterize the p-1,2-DAAQ/Au modified electrode. Factors such as the polymer film thickness, electrolyte, square wave parameters and preconcentration conditions were optimized to improve the performance of the modified Au electrode. Good linear responses were achieved in the concentration ranges of 1–200 μg L−1 and 1–50 μg L−1 forBi3+ and Hg2+, respectively, and the limits of detection were 0.27 μg L−1 (Bi3+) and 0.29 μg L−1 (Hg2+). The interference study results illustrated the high selectivity of the modified electrode for detection of Bi3+ and Hg2+. The proposed SW-ASV method was successfully applied for Bi3+ and Hg2+analyses in different real water samples.  相似文献   

11.
《Electroanalysis》2018,30(9):2004-2010
The performance of screen‐printed electrodes modified in situ with tellurium film for the anodic stripping voltammetric (ASV) determination of Cu(II) is reported. It was found that two types of screen‐printed substrates, namely carbon and mesoporous carbon, were optimal for this application. The selected in situ tellurium film modified electrodes were applied for the square wave ASV determination of copper at μg L−1 concentration levels. Well‐defined and reproducible Cu oxidation stripping peaks were produced at a potential more negative than the anodic dissolution of tellurium. The highest sensitivity of Cu determination was achieved in 0.05 M HCl containing 50 μg L−1 Te(IV) after 300 s of accumulation at −0.5 V. Using the optimized procedure, a linear range from 2 to 35 μg L−1 of Cu(II) was obtained with a detection limit of 0.5 μg L−1 Cu(II) (S/N=3) for 300 s of deposition time. Both sensors, carbon TeF‐SPE and mesoporous carbon TeF‐SPE, were successfully applied for the quantification of Cu in a certified reference surface water sample.  相似文献   

12.
Two sensitive and selective potentiometric sensors based on zinc-iron layered double hydroxides/multiwalled carbon nanotubes (Zn−Fe LDH/MWCNTs) (sensor I) and graphene/multiwalled carbon nanotubes (Gr/MWCNTs) (sensor II) nanocomposites were developed for benzydamine hydrochloride (Benz) determination. The investigated sensors displayed excellent Nernstian slopes 58.5±0.7 and 59.5±0.5 mV decade−1, detection limits 8.3×10−7 and 1.9×10−7 mol L−1, long lifetimes, adequate selectivity, high chemical, and thermal stability within pH range of 2.4–8.5 for sensors І and ІІ, respectively. The surface morphology of sensors was analyzed using a Transmission Electron Microscope (TEM). The analytical method was efficiently implemented for Benz determination in biological fluids and surface water samples.  相似文献   

13.
《Electroanalysis》2017,29(4):1069-1080
In this study, we introduce a very sensitive and selective method for the differential pulse anodic stripping determination of Sb(III) ion on the over‐oxidized poly(phenol red) modified glassy carbon electrode (PPhRedox/GCE) in 0.1 mol L‐1 HCl medium. The formation of both poly(phenol red) and over‐oxidized poly(phenol red) film on the electrode surfaces were characterized by electrochemical impedance spectroscopy, X‐ray photoelectron spectroscopy and scanning electron microscopy techniques. An anodic stripping peak of Sb(III) was observed at 0.015 V on the PPhRedox/GCE. Higher anodic stripping peak current of Sb(III) was obtained at PPhRedox/GCE compared with both bare GCE and poly(phenol red) film modified GCE (PPhRed/GCE). The calibration graph consisted of two linear segments of 0.044 ‐ 1.218 μg L−1 and 3.40 – 18.26 μg L−1 with a detection limit of 0.0075 μg L−1. The proposed over‐oxidized polymer film modified electrode was applied successfully for the analysis of antimony in different spiked water samples. Spiked recoveries for water samples were obtained in the range of 93.0–103.0%. The accuracy of the method was also verified through the analysis of standard reference materials (SCP SCIENCE‐EnviroMAT™ EP−L‐2).  相似文献   

14.
Herein, co-electrodeposition of AuNPs and ERGO onto GCE was conducted to prepare the modified electrode, GCE/AuNPs-ERGO. The poly(indole-5-carboxylic acid) (P(In-5-COOH) was then coated onto the GCE/AuNPs-ERGO with the help of electropolymerization. FT-IR, FE-SEM and EDX, and XRD techniques were employed to characterize the prepared nanocomposite. The nanocomposite modified electrode (GCE/AuNPs-ERGO/P(In-5-COOH)) was examined for the electrochemical reduction of H2O2 using chronoamperometry. A high reduction current for H2O2 was observed due to the synergistic effect between AuNPs-ERGO and P(In-5-COOH). The proposed sensor demonstrated a wide linear range of 0.025–750 μmol L−1, with a LOD of 0.008 μmol L−1 at −0.4 V. Furthermore, the developed sensor was applied for the detection of H2O2 in fetal bovine serum and urine samples.  相似文献   

15.

The two adsorptive stripping voltammetric approaches for detection and quantitative determination of diethyl (2E)-2-{(2E)-[1-(4-methylphenyl)imidazolidin-2-ylidene]hydrazinylidene}butanedioate (DIB)—a novel molecule of medical importance—using two sensitive sensors based on modified glassy carbon electrodes as reusable sensors, were developed for the first time. The proposed electrochemical methods are based on adsorptive/reductive behaviour of DIB at two modified carbonic electrodes: a bismuth film-modified glassy carbon electrode (BiF/GCE) and a lead film-modified glassy carbon electrode (PbF/GCE). The electron gain mechanism for the electrochemical reduction of DIB on both developed sensors was proposed for the first time. To achieve the highest sensitivity in adsorptive stripping determinations, various experimental variables (e.g. the composition and pH of the supporting electrolytes, deposition conditions of bismuth and lead films, concentrations of plating solutions, accumulation times and potentials of DIB, etc.) were extensively examined. The comparison of validation parameters obtained during the determination of DIB at two sensors was presented. The excellent linear correlation was found between the monitored adsorptive stripping voltammetric peak current and the DIB concentration in the range of 15–600 μg L−1 at an accumulation time of 30 s (with LOD = 4.2 μg L−1 and LOQ = 14.0 μg L−1) using the BiF/GCE as a sensor. Furthermore, the excellent linear relationship was confirmed between the monitored adsorptive stripping voltammetric peak current and the DIB concentration in the range of 9–900 μg L−1 at an accumulation time of 10 s (with better LOD = 1.5 μg L−1 and LOQ = 5.0 μg L−1), employing the PbF/GCE as a sensor. The two optimized adsorptive stripping voltammetric approaches—as facile, sensitive, reliable and inexpensive—were successfully used as first methods for the quantitative analysis of a novel anticancer agent (DIB) in its pure pharmaceutically acceptable form. However, the practical applicability of square-wave adsorptive stripping voltammetric determination of the electroactive DIB molecule at a PbF/GCE, as the modified electrode of higher sensitivity, was presented after its successful solid phase extraction from a real serum sample.

  相似文献   

16.
Capacitive deionization is a promising technique in sea water desalination. Compared with common electrodes, mixed capacitive-deionization electrodes exhibit better performance in sea water desalination because they integrate pseudocapacitance and electric double-layer capacitance in one system. Herein, a 3D binder-free mixed capacitive-deionization electrode was fabricated by direct electrodeposition of SiW12O404− and polyaniline on a 3D exfoliated graphite carrier. In this electrode, SiW12O404−/polyaniline composite particles with a size of about 100–120 nm are dispersed homogenously on the 3D exfoliated graphite carrier. Its specific capacitance reaches 352 F g−1 at 1 A g−1. With increasing current from 1 to 20 A g−1, the specific capacitance only decays by 32 %. When employed in sea water desalination, the performance of this mixed capacitive-deionization electrode is also excellent. At 1.2 V, the salt adsorption capacity of this mixed electrode reaches 23.1 mg g−1 with a salt adsorption rate of 1.38 mg g−1 min−1 in 500 mg L−1 NaCl. The performance of this electrode is well retained after 30 cycles. The excellent sea water desalination performance originates from the synergistic effect between SiW12O404− and polyaniline. This work has developed polyoxometalate as a new material for capacitive-deionization electrodes.  相似文献   

17.
We report a new strategy for efficient removal of F? from contaminated water streams, and it relies on carbon hybrid membranes made of amyloid fibril/ZrO2 nanoparticles (<10 nm). These membranes exhibit superior selectivity for F? against various competitive ions, with a distribution coefficient (Kd) as high as 6820 mL g?1, exceeding commercial ion‐exchange resins (IRA‐900) by 180 times and outdoing the performance of most commercial carbon‐activated aluminum membranes. At both low and high (ca. 200 mg L?1) F? concentrations, the membrane efficiency exceeds 99.5 % removal. For real untreated municipal tap water (ca. 2.8 mg L?1) under continuous operating mode, data indicates that about 1750 kg water m?2 membrane can be treated while maintaining drinking water quality, and the saturated membranes can be regenerated and reused several times without decrease in performance. This technology is promising for mitigating the problem of fluoride water contamination worldwide.  相似文献   

18.
Carbon Paste Electrodes (CPE) modified with Grapefruit-Peels (GP) functionalized with Urea (GPU) and, Melamine (GPM) were designed for the detection of Ag+ in water. Taguchi L9 methodology was used to determine the optimal graphite-Active material ratio. The best electrochemical response was for CPE-GPU with an 80 : 20 ratio. The results obtained showed a linear detection range between 0.5 to 28 μg L−1, with a detection limit of 0.73 μg L−1 and a limit of quantification of 1.04 μg L−1. Attributable to CPE-GPU characteristics: electroactive surface area 0.175 cm2, roughness factor 3.87, resistance 0.09 Ω and, mostly −NH2 groups on its surface. The composite material offers a viable option to be used for the determination of silver traces in situ in industrial processes.  相似文献   

19.
《Electroanalysis》2018,30(9):2176-2184
The contamination of water and wastewater by emerging pollutants, due to the anthropogenic activities, are an environmental problem that generates several negative impacts. In this range of species, steroids have gaining notoriety because their action of endocrine‐disruption. In this work, they are called estrogenic phenolic compounds (EPCs): estrone (E1), estradiol (E2), ethinyl estradiol (EE2) and estriol (E3), for determination using an electrochemical sensor based on reduced graphene oxide (rGO) and molecularly imprinted polymer (MIP). The analytical method developed, allied with the experimental and operational optimizations, proved to be effective for the total quantification of the EPCs in river water. The method shows sensitivity of 1.12 μA/μmol L−1, detection limit of 26.8 nmol L−1 and linear range of 0.16–15 μmol L−1. The similar electrochemical behavior of the four compounds studied (E1, E2, EE2 and E3) and the efficiency of the modified composite (rGO, MIP) in the fabrication of the sensor resulted in high electrical conductivity and selective adsorptivity, respectively.  相似文献   

20.
Cortisol is a steroid hormone naturally produced by the adrenal glands. It participates in and controls several processes in the body and is considered an important physiological biomarker. Due to its very low concentrations in body fluids, its detection requires high sensitivity and specificity. Here, we present a simple electrochemical biosensor based on reduced graphene oxide (rGO) modified with gold nanoparticles (AuNPs) for the immobilization of the cortisol-specific aptamer (Ap) (MCH-Ap-AurGO/GCE). Important analytical parameters for identifying the target analyte were optimized, such as conditions and amount of immobilized Ap, the influence of the concentration and nature of the supporting electrolyte, pH of the medium, and incubation time. The optimized conditions for the aptasensor were: concentration of Ap 1.0 × 10−6 mol L−1, support electrolyte Tris/HCl 50 mmol L−1, MgCl2 10 mmol L−1, and NaCl 10 mmol L−1, at pH 5.0 and incubation time of 15 min. A linear response range was obtained from 1 × 10−18 up to 1 × 10−11 mol L−1 of cortisol with a detection limit (LOD) of 1.0 × 10−18 mol L−1. A curve adjusted for operational purposes in the saliva sample was fitted for the concentration range between 0.5 × 10−14 and 1 × 10−11 mol L−1, with a linear regression equation ΔRtc/Rtc1 = 2.70 + 0.17 × log([Cortisol]). The aptasensor demonstrated a great potential for detecting cortisol in a simple, fast, and highly sensitive way, opening its path for application in real samples, which present levels below the concentration in which cortisol is commonly found in body fluids.  相似文献   

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