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1.
A novel silsesquioxane and cobalt nitroprusside compound was prepared from octa(aminopropyl)silsesquioxane, resulting in a nanocomposite (ACCoN), which was then characterized by different spectroscopic techniques. The cyclic voltammograms of the ACCoN-modified graphite paste electrode indicated a redox pair with a formal potential (Eθ′)=0.38 V, assigned to the Co(II)Fe(II)(CN)5NO/Co(II)Fe(III)(CN)5NO redox couple. The ACCoN-modified graphite paste electrode was sensitive to isoniazid concentrations, presenting a linear response at a concentration range from 6.0×10−7 to 1.0×10−5 mol L−1, with limit of detection and amperometric sensitivity of 5.53×10−7 mol L−1 and 0.17 A/mol L−1, respectively.  相似文献   

2.
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   

3.
This work describes the development of a fast, precise and reliable voltammetric method for the quantification of indapamide, an orally active diuretic sulfonamide used for hypertensive treatment. This compound acts inhibiting sodium reabsorption and increasing the elimination of water. This characteristic was responsible for its banishment by the International Olympic Committee since 1999. The study begins by finding an adequate potential range (−0.20 to 0.30 V) to avoid poisoning the working glassy carbon electrode (GCE) in phosphate buffer 0.10 mol L−1 (pH=12.0). Utilizing flow injection analysis, linear responses between 2.0 × 10−6 mol L−1 to 2.5 × 10−5 mol L−1 of indapamide (R2=0.995), and detection limit (LOD) 3.0 × 10−7 mol L−1 were obtained. This method was applied for the quantification of indapamide in tablets and in synthetic urine. The same flow system was used for the analysis of commercial drugs and the response obtained corresponded to 98 % of the concentration indicated on the drug label. These tablets were also analyzed by high performance liquid chromatography (HPLC), obtaining a recovery of 103 % and LOD 4.0 × 10−7 mol L−1. The velocity of analysis using flow methods compares advantageously to the classical chromatographic methods. For synthetic urine, linear responses were obtained in samples spiked in the region from 5.0 × 10−6 mol L−1 to 30 × 10−6 mol L−1 (R2=0.991) and LOD 3.0 × 10−7 mol L−1.  相似文献   

4.
This study reports a comparison of adsorptive transfer and solution phase voltammetric methods for the study of caffeic acid. For this purpose, a platform was prepared by the modification of glassy carbon electrodes (GCEs) with MWCNTs and samarium nanoparticles (SmNPs) by means of an ultrasonic bath. The surface morphology of the platform was characterized using SEM, EDX and XRD. The adsorptive transfer voltammetric method was based on the adsorption of caffeic acid (CFA) at the surface of the modified electrode by keeping it into a solution of CFA. Afterwards, the modified electrode was transferred with the adsorbed species in a cell containing only 0.1 mol L−1 phosphate buffer solution (PBS) for the analysis. The current response of CFA was found to be linear over a concentration from 5.0 × 10−10 mol L−1 to 1.0 × 10−7 mol L−1. The values of the limit of detection (LOD) and limit of quantification (LOQ) were 2.0 × 10−10 mol L−1 and 6.67 × 10−10 mol L−1, respectively. The adsorptive transfer method using the modified electrode (SmNPs/MWCNTs/GCE) has successfully been applied to food samples for determining CFA. The solution phase voltammetry was carried out by dipping the electrode into a voltammetric cell containing CFA. The plot of peak currents was linear over the concentration range of 5.0 × 10−9 mol L−1 –8.0 × 10−8 mol L−1. The values of LOD and LOQ were 2.0 × 10−9 mol L−1 and 6.67 × 10−9 mol L−1 for CFA using a classical solution phase voltammetry at the proposed platform. It was shown that the LOD obtained at adsorptive transfer voltammetry was 10-fold lower when compared to classical solution phase voltammetry.  相似文献   

5.
《Electroanalysis》2018,30(1):101-108
The present work describes the evaluation of microfluidic electroanalytical devices constructed by a 3D printer using ABS (acrylonitrile butadiene styrene) polymer combined with cotton threads as microchannels. Screen‐printed carbon electrodes (SPCEs) were used as electrochemical detector for amperometric determination of gallic and caffeic acid in wine samples. Using optimal experimental conditions (flow rate of 0.71 μL s−1, applied potential of +0.30 V and volume of injection of 2.0 μL) the proposed method presented a linear response for a concentration range of 5.0×10−6 to 1.0×10−3 mol L−1. The detection limits for gallic and caffeic acid were found to 1.5×10−6 mol L−1 and 8.0×10−7 mol L−1, respectively, with a sample throughput of 43 h−1. The achieved results are in agreement with those found using the official Folin‐Ciocaulteu method.  相似文献   

6.
《Electroanalysis》2017,29(5):1459-1468
A UO22+‐PVC membrane electrode was constructed using 2‐thenoyltrifluoroacetone as ionophore and its electrochemical response performance was characterized. The effect of membrane composition on the electrode performance was studied and best results were obtained using dioctylsebacate as a mediator and potassium tetrakis(4‐chlorophenyl)borate as anion excluder. The optimized UO22+‐sensor exhibited a Nernstian response with a slope of 29.5±0.5 mV decade−1 over the concentration range 5.0×10−7−1.0×10−1 mol L−1 at 25 °C with a detection limit of 3.1×10−7 mol L−1. The optimized electrode showed very good selectivity towards UO22+ relative to a wide variety of other cations and fast response time. Surface morphology of the optimized membrane electrode at different stages of its development and use was investigated and discussed. Quantum chemical calculations for geometrical optimization of the ionophore were carried out to investigate the interaction between the ionophore and UO22+ using DFT B3LYP/6‐31++G(d,p) level of theory and the obtained data confirmed the proposed response mechanism. The developed sensor was successfully applied for UO22+ selective determination in real water samples and the obtained results were compared to those obtained by spectrophotometric method indicating no significant difference.  相似文献   

7.
In the present work, a novel sensitive electrochemical potentiometric sensor for sensing Fe3+ ions based on 1,4-diaminoanthraquinone (DAQ) as a hydrophobic selector element was prepared to implement as an ion selective carbon paste electrode in the aqueous solutions. The adequate amounts of ionophore (5%), paraffin oil (25%) as a binder, Nanosilica (NS: 0.5%) multi-wall carbon nanotubes (MWCNTs: 1%) as a modifier, and graphite powder (68.5%) as an inert matrix was occupied to form the paste. This new FeCP sensor demonstrated a Nernstian slope of 19.7 ± 0.7 mV per decade over widish linear range between 1.0 × 10–8 to 1.0 × 10–2 mol L–1 at working pH range of 1.9–5.0 in the optimized conditions. The average elapsed time to response of electrode was about ~6 s for concentrations from lower (1.0 × 10?8 mol L–1) to higher (1.0 × 10?2 mol L–1) of Fe3+ ion solution. The selectivity of electrode toward Fe3+ ions in comparison with other cations was studied by matched potential method. The making FeCP sensor has been put to use successfully as an indicator electrode in analytical applications such as the potentiometric titration and determination of iron(III) ion in blend of different ions.  相似文献   

8.
采用噻唑蓝(MTT)法、碱性磷酸酶(ALP)比活性测定、油红O染色和茜素红染色及定量分析,研究了不同浓度的Fe3+和Fe2+对原代培养的成骨细胞增殖、分化及矿化功能的影响.结果表明:浓度为1×10-9~1×10-4 mol·L-1的Fe3+和Fe2+促进成骨细胞增殖,但是在较高浓度1×10-3 mol·L-1时,它们则抑制成骨细胞增殖.与成骨细胞作用48 h,浓度为1×10-8~1×10-4 mol·L-1的Fe3+和Fe2+抑制其分化,但在较低的浓度1×10-9 mol·L-1时则对其分化没有影响:进一步延长作用时间为72 h,Fe3+对成骨细胞分化没有影响,除1×10-6mol·L-1浓度的Fe2+促进成骨细胞分化外,其他浓度的Fe2+则抑制其分化;测试浓度下的Fe3+对成骨细胞向脂肪细胞的横向分化表现为抑制或没有影响,而Fe2+的影响则依赖于浓度和作用时间.在1×10-8~1×10-5mol·L-1浓度范围内,Fe3+和Fe2+对矿化结节的影响表现出相反的效应.在较高浓度(1×10-4mol·L-1)下,它们促进矿化节结的形成,而在较低浓度(1×10-9mol·L-1)下,Fe3+抑制矿化节结的形成,Fe2+则没有影响.结果提示:浓度.作用时间和铁离子的价态都是影响Fe3+和Fe2+生物效应(从毒性到活性,从损伤到保护,从上调到下调)转变的关键因素.  相似文献   

9.
In this work, a renewable tyrosinase-based biosensor was developed for the detection of catechol, using a carbon black paste electrode, without any mediator. The effect of pH, type of electrolyte, and amount of tyrosinase enzyme were explored for optimum analytical performance. The best-performing biosensor in amperometric experiments at potential −0.2 V vs. Ag/AgCl (3 mol L−1 KCl) was obtained using a 0.1 mol L−1 phosphate buffer solution (pH 7.0) as electrolyte. Under optimized conditions, the proposed biosensor had two concentration linear ranges from 5.0×10−9 to 4.8×10−8 and from 4.8×10−8 to 8.5×10−6 mol L−1 and a limit of detection of 1.5×10−9 mol L−1. The apparent Michaelis-Menten constant ( ) was calculated by the amperometric method, and the obtained value was 1.2×10−5 mol L−1 whose result was similar when compared with other studies previously. The biosensor was applied in river water samples, and the results were very satisfactory, with recoveries near 100 %. In addition, the response of this biosensor for different compounds, taking into account their molecular structures was investigated and the results obtained showed no interference with the response potential of catechol. The electrochemical biosensor developed in this work can be considered highly advantageous because it does not require the use of a mediator (direct detection) for electrochemical response, and also because it is based on a low-cost materials that can be used with success to immobilise other enzymes and/or biomolecules.  相似文献   

10.
An effective electrochemical sensor was constructed using an unmodified boron-doped diamond electrode for determination of genistein by square-wave voltammetry. Cyclic voltammetric investigations of genistein with HClO4 solution indicated that irreversible behavior, adsorption-controlled and well-defined two oxidation peaks at about +0.92 (PA1) & +1.27 V (PA2). pH, as well as supporting electrolytes, are important in genistein oxidations. Quantification analyses of genistein were conducted using its two oxidation peaks. Using optimized experiments as well as instrumental conditions, the current response with genistein was proportionately linear in the concentrations range of 0.1 to 50.0 μg mL−1 (3.7×10−7−1.9×10−4 mol L−1), by the detection limit of 0.023 μg mL−1 (8.5×10−8 mol L−1) for PA1 and 0.028 μg mL−1 (1.1×10−7 mol L−1) for PA2 in 0.1 mol L−1 HClO4 solution (in the open circuit condition at 30 s accumulation time). Ultimately, the developed method was effectively applied to detect genistein in model human urine samples by using its second oxidation peak (PA2).  相似文献   

11.
This article describes a method that uses Carbon Screen-printed Electrodes (C-SPEs) to detect 3,4 – methylenedioxyamphetamine (MDMA) by Linear Sweep Voltammetry in aqueous medium. Major parameters of this technique were evaluated aiming improve the method sensibility. Amines interference were conducted in order to verify disturbs at the MDMA response. The method obtained a linear response from 1×10−5 mol L−1 to 1×10−4 mol L−1 with linear correlation coefficient of 0.996, Amperometric Sensitivity (AS) of 0.025 A×mol−1 L, Limit of Detection (LOD) of 1,83×10−6 mol L−1, and Limit of Quantification (LOQ) of 6,11×10−6 mol L−1. The method applicability, reproducibility and reproducibility were carried over inter/intra days tests and its application on seized samples.  相似文献   

12.
《Electroanalysis》2017,29(2):441-447
A convenient and simple electrochemiluminescence (ECL) method was employed to detect trace amounts of Cu2+ in drinking water. This method is based on the inhibitory effect of Cu2+ on the ECL of Ru(phen)32+ and 1,4,8,11‐tetraazacyclotetradecane (cyclam) system. ECL intensity of Ru(phen)32+ was considerably enhanced by the addition of cyclam because of the ECL reaction between them. The ECL intensity of Ru(phen)32+/cyclam system rapidy decreased with the addition Cu2+ because of the formation of chelate complex [Cu(cyclam)]2+. Good linear response (R 2=0.9948) was obtained at Cu2+ concentration of 1.0×10−9−1.0×10−5 mol ⋅ L−1 at glassy carbon electrode in 0.1 mol ⋅ L−1 phosphate buffer (pH 9.0). Observed detection limit of 4.8×10−10 mol ⋅ L−1 satisfied the maximum contaminant level goal (MCLG) for Cu2+ set by the US Environmental Protection Agency (US EPA). Applicability of the proposed method was verified by the good reproducibility and stability of the method when applied to determine Cu2+ in tap water and simulated wastewater. Thus, a novel ECL detection method was developed for Cu2+ detection.  相似文献   

13.
A novel chemiluminescence (CL) method for the determination of hydrogen peroxide is described. Method is based on the transition metals in highest oxidation state complex, which include diperiodatoargentate (DPA) and diperiodatonickelate (DPN) and show excellent sensitisation on the luminol-H2O2 CL reaction with low luminol concentration in alkaline medium. In particular, the sensitiser which was previously reported (such as Co2+, Cu2+, Ni2+, Mn2+, Fe3+, Cr3+, KIO4, K3Fe(CN)6 etc.) to be unobserved CL due to poor sensitisation with such low concentration of luminol which makes the method hold high selectivity. Based on this observation, the detection limits were 6.5?×?10?9?mol?L?1 and 1.1?×?10?8?mol?L?1 hydrogen peroxide for the DPN- and DPA-luminol CL systems, respectively. The relative CL intensity was linear with the hydrogen peroxide concentration in the range of 2.0?×?10?8–6.0?×?10?6?mol?L?1 and 4.0?×?10?8–4.0?×?10?6?mol?L?1 for the DPN- and DPA-luminol CL systems, respectively. The proposed method had good reproducibility with a relative standard deviation of 3.4% (8.0?×?10?7?mol?L?1, n?=?7) and 1.0% (2.0?×?10?6?mol?L?1, n?=?7) for the DPN- and DPA-luminol CL systems, respectively. A satisfactory result has been gained for the determination of H2O2 in rainwater and artificial lake water by use of the proposed method.  相似文献   

14.
《Electroanalysis》2017,29(4):1154-1160
Oxidation and reduction processes of the insecticide fenthion was comparatively investigated at a reduced graphene oxide modified glassy carbon electrode (RGO‐GCE) and a cyclic renewable silver amalgam film electrode (Hg(Ag)FE) using square wave stripping voltammetry (SWSV). The influence of pH and SW parameters was investigated. The linear concentration ranges were found to be 1 × 10−6 – 2 × 10−5 and 1 × 10−7 – 2 × 10−5 mol L−1 for Hg(Ag)FE and RGO‐GCE, respectively. The detection and quantification limits were calculated as 1.3 × 10−7 and 4.5 × 10−7 mol L−1 for Hg(Ag)FE and 7.6 × 10−9 and 2.5 × 10−8 mol L−1 for RGO‐GCE. Both of the developed electroanalytical methods offer rapid and simple detection of fenthion and were used on spiked tap and river water and apple juice samples. Scanning electron microscopy was used for RGO‐GCE surface characterization.  相似文献   

15.
Iwona Gęca 《Electroanalysis》2023,35(3):e202200256
An anodic stripping voltammetric procedure for the determination of bismuth in the presence of excess of Cu2+ ions at two ex situ plated gold film electrodes was described. The procedure is based on utilization of two deposition and two stripping steps system. The presented procedure ensures increasing the sensitivity of Bi3+ determination and minimization of interferences related to peaks’ overlapping. The calibration graph for bismuth determination was linear from 2.5×10−9 to 2×10−8 mol L−1 for deposition time of 300 s at both working electrodes while detection limit was 7.7×10−10 mol L−1.  相似文献   

16.
The removal of heavy metal ions from water using electron beam and gamma irradiation has been investigated for the cases of Pb2+ and Hg2+ ions. These metal ions are reduced by hydrated electrons and hydrogen atoms to lower or zero valence state and eventually precipitate out of solution. Ethanol is applied as a relatively non-toxic additive to scavenge ·OH radicals, to enhance reduction and inhibit oxidation. Mercury can be completely (>99.9%) removed from aqueous solution of 1×10−3 mol L−1 mercury (II) chloride by using a 3 kGy dose. However, a 40 kGy dose is required to remove 96% of lead ions from a 1×10−3 mol L−1 of PbCl2 solution. The effect of dissolved oxygen and carbonate were also investigated. E-beam irradiation of 1×10−3 mol L−1 lead ions complexed with ethylenediamine tetraacetic acid (EDTA) in deoxygenated as well as air-saturated solutions in the absence of ethanol resulted in removal of about 97% of the lead.  相似文献   

17.
This work presents the analytical method development for iron and copper determination in ethanol fuel. This method was developed using stripping voltammetry with a glassy carbon electrode modified with Nafion/Carbon‐nanotubes. With linear sweep stripping voltammetry was achieved a limit of detection of 7.1×10?7 mol L?1 for Fe3+ and 5.1×10?8 mol L?1 for Cu2+. The amperometric sensitivities were 2.0×106 µA mol?1 L for Fe3+ and 2.8×107 µA mol?1 L for Cu2+. The recovery study showed that the method has good accuracy and repeatability, with recovery of 108 and 103 % for Fe3+ and Cu2+ respectively.  相似文献   

18.
《Electroanalysis》2017,29(11):2579-2590
In this study, an electrochemical sensor was developed and used for selective determination of bisfenol‐A (BPA) by integrating sol‐gel technique and multi‐walled carbon nanotubes (MWCNTs) modified paste electrode. BPA bounded by covalently to isocyanatopropyl‐triethoxy silane (ICPTS) was synthesized as a new precursor (BPA‐ICPTS) and then BPA‐imprinted polymer (BPA‐IP) sol‐gel was prepared by using tetramethoxysilane (TMOS) and BPA‐ICPTS. Non‐imprinted polymer (NIP) sol‐gel was obtained by using TMOS and (3‐Aminopropyl) triethoxysilane. Both BPA‐IP and NIP sol‐gels were characterized by nitrogen adsorption‐desorption analysis, FTIR, SEM, particle size analyzer and optical microscope. Carbon paste sensor electrode was fabricated by mixing the newly synthesized BPA‐IP with MWCNTs, graphite powder and paraffin oil. The electrochemical characterization of the sensor electrode was achieved with cyclic and differential pulse voltammetric techniques. The response of the developed sensor under the most proper conditions was linear in BPA concentration range from 4.0×10−9 to 1.0×10−7 mol L−1 and 5.0×10−7 to 5.0×10−5 mol L−1 and the detection limit was 4.4×10−9 mol L−1. The results unclosed that the proposed sensor displayed high sensitivity and selectivity, superior electrochemical performance and rapid response to BPA.  相似文献   

19.
《Electroanalysis》2017,29(7):1691-1699
The simultaneous voltammetric determination of melatonin (MT) and pyridoxine (PY) has been carried out at a cathodically pretreated boron‐doped diamond electrode. By using cyclic voltammetry, a separation of the oxidation peak potentials of both compounds present in mixture was about 0.47 V in Britton‐Robinson buffer, pH 2. The results obtained by square‐wave voltammetry allowed a method to be developed for determination of MT and PY simultaneously in the ranges 1–100 μg mL−1 (4.3×10−6–4.3×10−4 mol L−1) and 10–175 μg mL−1 (4.9×10−5–8.5×10−4 mol L−1), with detection limits of 0.14 μg mL−1 (6.0×10−7 mol L−1) and 1.35 μg mL−1 (6.6×10−6 mol L−1), respectively. The proposed method was successfully to the dietary supplements samples containing these compounds for health‐caring purposes.  相似文献   

20.
《Electroanalysis》2017,29(2):566-577
Two novel carbon paste electrodes based on gentamicin‐reineckate (GNS‐RN)/multiwall carbon nanotubes (MWCNTs)/sodium tetraphenyl borate (NaTPB) or potassium tetraphenylborate (KTPB) for potentiometric determination of gentamicin sulfate were constructed. Our endeavors of lowering the detection limit for gentamicin ion‐selective electrodes were described. The paper focused on gentamicin carbon paste electrodes based on GNS‐RN as electroactive material, o ‐nitrophenyloctyl ether (o ‐NPOE) as plasticizer and incorporation of MWCNTs and lipophilic anionic additives (NaTPB and KTPB) which lower the detection limit of the electrodes showing best results for determination of gentamicin ion. The characteristics of the electrodes, GNS‐RN+NaTPB+MWCNTs (sensor 1) and GNS‐RN+KTPB+ MWCNTs (sensor 2), were measured, showing favorable features as they provided measurements of the potential with near‐Nernstian slopes of 29.6±0.3 and 29.1±0.3 mV/decade over the concentration range of 1.0×10−6–1.0×10−2 mol L−1 and pH ranges 3.0–8.2 and 3.0–8.0 in short response times (6.5 sec). Importantly, the electrodes had low detection limits of 3.0×10−7and 3.4×10−7 mol L−1 for the two sensors, respectively. The sensors showed high selectivity for gentamicin ion with respect to a large number of interfering species. The electrodes were successfully applied for the potentiometric determination of GNS ions in pure state, pharmaceutical preparations and human urine with high accuracy and precision. The results of this study were compared with some previously published data using other analytical methods.  相似文献   

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