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1.
A method for determination of nine brominated phenols as environmental risk compounds was developed by on-line coupled capillary isotachophoresis and capillary zone electrophoresis (ITP–CZE). For ITP step, 1 × 10−2 mol L−1 hydrochloric acid with 3 × 10−2 mol L−1 ammediol pH 9.1 was used as the leading electrolyte, and 3 × 10−2 mol L−1 β-alanine with 2 × 10−2 mol L−1 sodium hydroxide pH 10.05 was used as the terminating electrolyte. As the background electrolyte for CZE separation, 2.5 × 10−2 mol L−1 β-alanine with 2.5 × 10−2 mol L−1 lysine pH 9.6 was used. All electrolytes contained 0.05% or 0.1% (m/v) hydroxyethylcellulose to suppress the electroosmotic flow. UV detection at wavelength 220 nm was used. Detection limits in order of tens of nmol L−1 were achieved. Good repeatability of migration times (less than 0.33% RSD) and good repeatability of peak areas (less than 7.19% RSD) at concentration level 5 × 10−8 mol L−1 were observed. Developed ITP–CZE method was applied to determination of brominated phenols in spiked tap and river water samples.  相似文献   

2.
A novel flow injection chemiluminescence (FI-CL) sensor for determination of sulfadiazine (SDZ) using core–shell magnetic molecularly imprinted polymers (MMIPs) as recognition element is developed. Briefly, a hydrophilic MMIPs layer was produced at the surface of Fe3O4@SiO2 magnetic nanoparticles (MNPs) via combination of molecular imprinting and reversible stimuli responsive hydrogel. And it provided the MMIPs with excellent adsorption capacity and rapid adsorption rate due to the imprinted sites mostly situated on the surface of MMIPs. Then the prepared SDZ-MMIPs were packed into flow cell to establish a novel FI-CL sensor. The sensor provided a wide linear range for SDZ of 4.0 × 10−7 to 1.0 × 10−4 mol L−1 with a detection limit of 1.54 × 10−7 mol L−1. And the relative standard deviation (RSD) for the determination of 1.0 × 10−6 mol L−1 SDZ was 2.56% (n = 11). The proposed method was applied to determine SDZ in urine samples and satisfactory results were obtained.  相似文献   

3.
A novel optical sensor based on a redox reaction for the determination of iodide has been developed. The optode membrane is constructed by immobilization of methyltrioctylammonium chloride on triacetylcellulose polymer. The exchange of chloride as counter ion with iodate in the membrane changes the color to yellow, when it is placed in acidic solution of iodide. The sensor can readily be regenerated by 0.1 mol L−1 NaOH in less than 15 s. The optode has a linear range of 3.94 × 10−6 to 5.51 × 10−5 mol L−1 of iodide ions with a limit of detection 7.44 × 10−7 mol L−1. The relative standard deviation for eight replicate measurements of 3.94 × 10−6 and 1.57 × 10−5 mol L−1 of iodide was 2.83 and 1.38%, respectively. The sensor was successfully applied to the determination of iodide in tablet, powdered milk and urine samples.  相似文献   

4.
A fluorometric method for quantity analysis of biothiols was developed using a graphene oxide (GO)-based “molecular beacon”-like probe, which consisted of FITC labeled thymine (T)-rich single-stranded DNA (ssDNA), GO and Hg2+ ions. The labeled ssDNA containing T–T mismatches would self-hybridize to duplex in the presence of Hg2+, which can avoid its adsorption on GO and the fluorescence of this GO-based probe was recovered. The fluorescence of the probe quenched after the addition of biothiols such as glutathione (GSH) and cysteine (Cys) owing to thiol groups can selectively competitive ligation of Hg2+ ions with T–T mismatches. In the present work, the GO-based probe was used for the determination of GSH and Cys. Under the optimal conditions, a linear correlation was established between fluorescence intensity ratio I0/I and the concentration of GSH in the range of 2.0 × 10−9–5.0 × 10−7 mol L−1 with a detection limit of 1.0 × 10−9 mol L−1. The linear range for Cys is from 5.0 × 10−9 to 4.5 × 10−7 mol L−1 with a detection limit of 2.0 × 10−9 mol L−1. The proposed method was applied to the determination of GSH in human serum and cell extract samples with satisfactory results.  相似文献   

5.
A novel method of first derivative synchronous fluorescence was developed for the rapid simultaneous analysis of trace 1-hydroxypyrene (1-OHP), 1-naphthol (1-NAP), 2-naphthol (2-NAP), 9-hydroxyphenanthrene (9-OHPe) and 2-hydroxyfluorene (2-OHFlu) in human urine. Only one single scan was needed for quantitative determination of five compounds simultaneously when Δλ = 10 nm was chosen. In the optimal experimental conditions, there was a linear relationship between the fluorescence intensity and the concentration of 1-OHP, 1-NAP, 2-NAP, 9-OHPe and 2-OHFlu in the range of 1.75 × 10−9 to 4.50 × 10−6 mol L−1, 3.64 × 10−8 to 2.20 × 10−4 mol L−1, 8.18 × 10−9 to 1.20 × 10−4 mol L−1, 3.26 × 10−9 to 8.50 × 10−5 mol L−1 and 4.88 × 10−9 to 5.50 × 10−6 mol L−1, respectively. The limits of detection (LOD) were found to be 5.25 × 10−10 mol L−1 for 1-OHP, 1.10 × 10−8 mol L−1 for 1-NAP, 2.46 × 10−9 mol L−1 for 2-NAP, 9.77 × 10−10 mol L−1 for 9-OHPe and 1.46 × 10−9 mol L−1 for 2-OHFlu. The proposed method is reliable, selective and sensitive, and has been used successfully in the determination of traces of 1-OHP, 1-NAP, 2-NAP, 9-OHPe and 2-OHFlu in human urine samples, whose results were in good agreement with those gained by the HPLC method.  相似文献   

6.
M.S. Attia  M.M. Aboaly 《Talanta》2010,82(1):78-33
A simple, sensitive and selective spectrofluorimetric method for the determination of Metoclopramide hydrochloride (MCP) is developed. The MCP can remarkably enhances the luminescence intensity of the Eu3+ ion doped in sol-gel matrix at λex = 380 nm in DMSO at pH 8.7. The intensity of the emission band of Eu3+ ion doped in sol-gel matrix increases due to energy transfer from MCP to Eu3+ in the excited state. The enhancement of the emission band of Eu3+ ion doped in sol-gel matrix at 617 nm was found to be directly proportional to the concentration of MCP with a dynamic range of 5 × 10−9 − 1.0 × 10−6 mol L−1 and detection limit of 2.2 × 10−11 mol L−1.  相似文献   

7.
The paper presents the first report on fabrication and application of a user friendly and mercury free electrochemical sensor, with the renewable bismuth bulk annular band working electrode (RBiABE), in stripping voltammetry (SV). The sensor body is partly filled with the internal electrolyte solution, in which the RBiABE is cleaned and activated before each measurement. Time of the RBiABE contact with the sample solution is precisely controlled. The usefulness of this sensor was tested by Ni(II) and Co(II) traces determination by means of differential pulse adsorptive stripping voltammetry (DP AdSV), after complexation with dimethylglyoxime (DMG) in ammonia buffer (pH 8.2). The experimental variables (composition of the supporting electrolyte, pre-concentration potential and time, potential of the RBiABE activation, and DP parameters), as well as possible interferences, were investigated. The linear calibration graphs for Ni(II) and Co(II), determined individually and together, in the range from 1 × 10−8 to 70 × 10−8 mol L−1 and from 1 × 10−9 to 70 × 10−9 mol L−1 respectively, were obtained. The calculated limit of detection (LOD), for 30 s of the accumulation time, was 3 × 10−9 mol L−1 for Ni(II) in case of a single element’s analysis, whereas the LOD was 5 × 10−9 mol L−1 for Ni(II) and 3 × 10−10 mol L−1 for Co(II), when both metal ions were measured together. The repeatability of the Ni(II) and Co(II) adsorptive stripping voltammetric signals obtained at the RBiABE were equal to 5.4% and 2.5%, respectively (n = 5). Finally, the proposed method was validated by determining Ni(II) and Co(II) in the certified reference waters (SPS-SW1 and SPS-SW2) with satisfactory results.  相似文献   

8.
By using a molecularly imprinted polymer (MIP) as a recognition element, the design and construction of a high selective voltammetric sensor for para-nitrophenol was formed. Para-nitrophenol selective MIP and a non-imprinted polymer (NIP) were synthesized, and then used for carbon paste (CP) electrode preparation. The MIP-CP electrode showed greater recognition ability in comparison to the NIP-CP. It was shown that electrode washing after para-nitrophenol extraction led to enhanced selectivity, without noticeably decreasing the sensitivity. Some parameters affecting sensor response were optimized and a calibration curve was plotted. A dynamic linear range of 8 × 10−9 to 5 × 10−6 mol L−1 was obtained. The detection limit of the sensor was calculated as 3 × 10−9 mol L−1. Thus, this sensor was used successfully for the para-nitrophenol determination in different water samples.  相似文献   

9.
Bisphenol A (BPA) is an emerging contaminant with severe toxic effects such as disrupting endocrine system or causing cancer, therefore, developing sensitive and selective sensor for BPA is very important and interesting. Herein, MCM-41, a kind of mesoporous silica, was synthesized and then used to prepare an electrochemical sensor for BPA. For better comparison, carbon nanotubes, activated carbon, silica gel and graphite were also employed to prepare electrochemical sensor for BPA. The electrochemical behaviors of BPA at different electrochemical sensors were investigated. Compared with other sensors, the MCM-41 sensor greatly enhances the response signal of BPA due to the large active surface area and high accumulation efficiency. The effects of pH value, accumulation time and sensor composition were examined. The linear range is from 2.2 × 10−7 to 8.8 × 10−6 mol L−1, and the limit of detection is evaluated to be 3.8 × 10−8 mol L−1. Finally, the MCM-41 sensor was successfully employed to determine BPA in water samples.  相似文献   

10.
Flow injection analysis (FIA) with amperometric detection was employed for the quantification of N-acetylcysteine (NAC) in pharmaceutical formulations, utilizing an ordinary pyrolytic graphite (OPG) electrode modified with cobalt phthalocyanine (CoPc). Cyclic voltammetry was used in preliminary studies to establish the best conditions for NAC analysis. In FIA-amperometric experiments the OPG-CoPc electrode exhibited sharp and reproducible current peaks over a wide linear working range (5.0 × 10−5-1.0 × 10−3 mol L−1) in 0.1 mol L−1 NaOH solution. High sensitivity (130 mA mol−1 cm2) and a low detection limit (9.0 × 10−7 mol L−1) were achieved using the sensor. The repeatability (R.S.D.%) for 13 successive flow injections of a solution containing 5.0 × 10−4 mol L−1 NAC was 1.1%. The new procedure was applied in analyses of commercial pharmaceutical products and the results were in excellent agreement with those obtained using the official titrimetric method. The proposed amperometric method is highly suitable for quality control analyses of NAC in pharmaceuticals since it is rapid, precise and requires much less work than the recommended titrimetric method.  相似文献   

11.
The influence of the boron-doping levels in boron-doped diamond film electrodes on the electrochemical response of nitrofurantoin (NFT) and the development of an electroanalytical procedure for NFT determination were investigated. The investigations were carried out using the techniques of cyclic voltammetry and square wave voltammetry on diamond film electrodes with different boron-doping levels (i.e., 5000, 10,000 and 20,000 mg L−1). The level of boron-doping in the diamond film electrodes influenced the electrochemical reduction of NFT. The appropriate cyclic voltammetric response of NFT was obtained with Britton-Robinson buffer at pH 4 and for diamond films doped with 10,000 and 20,000 mg L−1 of boron. These two films were selected for the development of the electroanalytical procedure. The use of square wave voltammetry with the optimized parameters demonstrated a good linear relationship between the peak current and the NFT concentration for a wide range of concentration. The lower limit of detection for the electrodes doped with 10,000 and 20,000 mg L−1 of boron were 2.69 × 10−8 mol L−1 (6.40 μg L−1) and 8.15 × 10−9 mol L−1 (1.94 μg L−1), respectively, while the lower limits of quantification were 8.96 × 10−8 mol L−1 (21.33 μg L−1) and 2.72 × 10−8 mol L−1 (6.47 μg L−1), respectively. The applicability of the proposed procedure was tested using a commercial pharmaceutical formulation of NFT, and the results were compared with the procedure recommended by the British Pharmacopeia. The proposed procedure was sensitive, accurate and precise for analysis of NFT and did not require complex preparations or renovations of the electrode surface. This presents the advantage of eliminating mercury waste and minimizing the adsorptive problems related to the use of other electrodic solid surfaces.  相似文献   

12.
A novel dual-function material was synthesized by anchoring a molecularly imprinted polymer (MIP) layer on CdTe/ZnS quantum dots (QDs) using a sol–gel with surface imprinting. The material exhibited highly selective and sensitive determination of ractopamine (RAC) through spectrofluorometry and solid-phase extraction (SPE) coupled with high performance liquid chromatography (HPLC). A series of adsorption experiments revealed that the material showed high selectivity, good adsorption capacity and a fast mass transfer rate. Fluorescence from the MIP-coated QDs was more strongly quenched by RAC than that of the non-imprinted polymer, which indicated that the MIP-coated QDs acted as a fluorescence sensing material could recognize RAC. In addition, the MIP-coated QDs as a sorbent was also shown to be promising for SPE coupled with HPLC for the determination of trace RAC in feeding stuffs and pork samples. Under optimal conditions, the spectrofluorometry and SPE-HPLC methods using the MIP-coated QDs had linear ranges of 5.00 × 10−10–3.55 × 10−7 and 1.50 × 10−10–8.90 × 10−8 mol L−1, respectively, with limits of detection of 1.47 × 10−10 and 8.30 × 10−11 mol L−1, the relative standard deviations for six repeat experiments of RAC (2.90 × 10−9 mol L−1) were below 2.83% and 7.11%.  相似文献   

13.
A facile and efficient molecularly imprinted polymer (MIP) recognition element of electrochemical sensor was fabricated by directly electro-polymerizing monomer o-phenylenediamine (oPD) in the presence of template quinoxaline-2-carboxylic acid (QCA), based on one-step controllable electrochemical modification of poly(pyrrole)-graphene oxide-binuclear phthalocyanine cobalt (II) sulphonate (PPY-GO-BiCoPc) functional composite on glassy carbon electrode (GCE). The MIP film coated on PPY-GO-BiCoPc functional composite decorated GCE (MIP/PPY-GO-BiCoPc/GCE) was presented for the first time. The synergistic effect and electro-catalytic activity toward QCA redox of PPY-GO-BiCoPc functional composite were discussed using various contrast tests. Also, the effect of experimental variables on the current response such as, electro-polymerization cycles, template/monomer ratio, elution condition for template removal, pH of the supporting electrolyte and accumulation time, were investigated in detail. Under the optimized conditions, the proposed MIP sensor possessed a fast rebinding dynamics and an excellent recognition capacity to QCA, while the anodic current response of square wave voltammetry (SWV) was well-proportional to the concentration of QCA in the range of 1.0 × 10−8–1.0 × 10−4 and 1.0 × 10−4–5.0 × 10−4 mol L−1 with a low detection limit of 2.1 nmol L−1. The established sensor was applied successfully to determine QCA in commercial pork and chicken muscle samples with acceptable recoveries (91.6–98.2%) and satisfactory precision (1.9–3.5% of SD), demonstrating a promising feature for applying the MIP sensor to the measurement of QCA in real samples.  相似文献   

14.
A novel voltammetric sensor for O,O-dimethyl-(2,4-dichlorophenoxyacetoxyl)(3′-nitrophenyl)methinephosphonate (Phi-NO2) based on molecularly imprinted polymer (MIP) film electrode is constructed by using sol-gel technology. The sensor responds linearly to Phi-NO2 over the concentration range of 2.0 × 10−5 to 1.0 × 10−8 mol L−1 and the detection limit is 1.0 × 10−9 mol L−1 (S/N = 3). This sensor provides an efficient way for eliminating interferences from coexisting substances in the solution. The high sensitivity, selectivity and stability of the sensor demonstrates its practical application for a simple and rapid determination of Phi-NO2 in cabbage samples.  相似文献   

15.
The carbazole derivative, 9-ethyl-3-carbazylidene carbazole hydrazone (ECCH) with two conjugated carbazole rings have been applied as a fluorescence carrier for preparation of an iodine sensitive optical chemical sensor. The response of the sensor is based on quenching of the fluorescence of ECCH by iodine. The conjugated carbazole dimer based sensor shows a linear response toward iodine in the concentration range 1.0 × 10−6 to 1.0 × 10−4 mol L−1, with a detection limit of 8.0 × 10−7 mol L−1 at pH of 7.0. The effect of composition of the sensor membrane was studied, and the experimental conditions were optimized. Most commonly coexisting ions do not interfer with the iodine assay. The sensor shows sufficient repeatability, selectivity, operational lifetime of two months and a fast response of less then 50 s. The sensor has been used for determination of iodine in water samples.  相似文献   

16.
17.
A new sensor for simultaneous determination of peroxyacetic acid and hydrogen peroxide using silver nanoparticles (Ag-NPs) as a chromogenic reagent is introduced. The silver nanoparticles have the catalytic ability for the decomposition of peroxyacetic acid and hydrogen peroxide; then the decomposition of them induces the degradation of silver nanoparticles. Hence, a remarkable change in the localized surface plasmon resonance absorbance strength could be observed. Spectra-kinetic approach and artificial neural network was applied for the simultaneous determination of peroxyacetic acid and hydrogen peroxide. Linear calibration graphs were obtained in the concentration range of (8.20 × 10−5 to 2.00 × 10−3 mol L−1) for peroxyacetic acid and (2.00 × 10−5 to 4.80 × 10−3 mol L−1) for hydrogen peroxide. The analytical performance of this sensor has been evaluated for the detection of simultaneous determination of peroxyacetic acid and hydrogen peroxide in real samples.  相似文献   

18.
Hu YF  Zhang ZH  Zhang HB  Luo LJ  Yao SZ 《Talanta》2011,84(2):305-313
A sensitive and selective electrochemical sensor based on a polyaniline modified carbon electrode for the determination of l-phenylalanine has been proposed by utilizing β-cyclodextrin (β-CD) incorporated multi-walled carbon nanotube (MWNT) and imprinted sol-gel film. The electrochemical behavior of the sensor towards l-phenylalanine was investigated by cyclic voltammetry (CV), differential pulse voltammetry (DPV), and amperometric i-t curve. The surface morphologies of layer-by-layer assembly electrodes were displayed by scanning electron microscope (SEM). The response mechanism of the imprinted sensor for l-phenylalanine was based on the inclusion interaction of β-CD and molecular recognition capacity of the imprinted film for l-phenylalanine. A linear calibration plot was obtained covering the concentration range from 5.0 × 10−7 to 1.0 × 10−4 mol L−1 with a detection limit of 1.0 × 10−9 mol L−1. With excellent sensitivity, selectivity, stability, reproducibility and recovery, the electrochemical imprinted sensor was used to detect l-phenylalanine in blood plasma samples successfully.  相似文献   

19.
A new heterodinuclear Fe(III)Zn(II) complex which mimics the active site of the hydrolytic enzyme red kidney bean purple acid phosphatase was synthesized and characterized by IR, CHN and X-ray crystallographic analyses. This complex, [FeIIIZnII(μ-OH)bpbpmp-CH3](ClO4)2, containing the ligand (H2bpbpmp-CH3 = {2-[bis(2-pyridylmethyl)aminomethyl]-6-[(2-hydroxy-5-methylbenzyl) (2-pyridyl-methyl) aminomethyl]-4-methyl-phenol}) was employed in the construction of a biomimetic sensor and used in the determination of rosmarinic acid in plant extract samples. The response parameters and optimization of the biomimetic sensor design were evaluated. The best performance of this sensor was obtained for 75:15:10% (w/w/w) of the graphite powder:nujol:Fe(III)Zn(II) complex, 0.1 mol L−1 phosphate buffer solution (pH 7.5), 1.19 × 10−4 mol L−1 hydrogen peroxide with frequency, pulse amplitude, and scan increment at 30 Hz, 100 mV, and 0.6 mV, respectively. The rosmarinic acid concentration was linear in the range of 2.98 × 10−5 to 3.83 × 10−4 mol L−1 (r = 0.9991) with a detection limit of 2.30 × 10−6 mol L−1. This biomimetic sensor demonstrated long-term stability (300 days; 900 determinations) and reproducibility, with a relative standard deviation of 12.0%. The recovery study of rosmarinic acid in plant extract samples gave values from 90.3 to 98.3% and the concentrations determined showed agreement when compared with those obtained using capillary electrophoresis at the 95% confidence level.  相似文献   

20.
An optical sensor for mercury ion (Hg2+), based on quenching the fluorescence of the sensing reagent porphyrin immobilized in plasticized poly(vinyl chloride) (PVC) membrane, has been developed. The responses to mercury ion were compared for the sensors modified with three porphyrin compounds including 5,10,15,20-tetraphenylporphyrin (TPP), tetra(p-dimethylaminophenyl)porphyrin (TDMAPP) and tetra(N-phenylpyrazole) porphyrin (TPPP). Among them, TDMAPP showed the most remarkable response to Hg2+. The drastic decrease of the TDMAPP fluorescence intensity was attributed to the formation of a complex between TDMAPP and Hg2+, which has been utilized as the fabrication basis of a Hg2+-sensitive fluorescence sensor. The analytical performance characteristics of the TDMAPP modified sensor was investigated. The response mechanism, especially involving the response difference of three porphyrin compounds, was discussed in detail. The sensor can be applied to the quantification of Hg2+ with a linear range covering from 4.0 × 10−8 mol L−1 to 4.0 × 10−6 mol L−1. The limit of detection was 8.0 × 10−9 mol L−1. The sensor exhibited excellent reproducibility, reversibility and selectivity. Also, the TDMAPP-based sensor was successfully used for the determination of Hg2+ in environmental water samples.  相似文献   

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