共查询到20条相似文献,搜索用时 31 毫秒
1.
A cathodic differential pulse voltammetric determination of colchicine was validated using a glassy carbon electrode in HClO4/H3PO4 0.01 M. Colchicine gives an irreversible, diffusion-controlled peak at −862 mV vs. Ag/AgCl reference electrode. The cathodic
peak is strongly influenced by a more alkaline environment with a shift towards more negative potentials. Method optimization
was carried out in parallel for three types of electrodes (glassy carbon, mercury film and bismuth film coated glassy carbon).
The cathodic peak current is higher using film-coated electrodes, but shows poorer intra-day reproducibility and a longer
analysis time due to film renewal. Thus, a bare glassy carbon electrode was used to determine colchicine in the concentration
range of 2.4 − 50 μg mL−1 (R
2 = 0.9998, n = 5), with a calculated detection limit of 0.80 μg mL−1. The proposed method was characterized according to ICH Harmonized Tripartite Guidance Q2(R1) by validation parameters (selectivity,
linearity, accuracy, fidelity, limit of detection, limit of quantification) and it was successfully applied for the determination
of colchicine from tablets, without the interference of the excipients. The method’s performances were evaluated and compared
with both a known polarographic method and the official quantitative spectrophotometric determination from the Romanian Pharmacopoeia,
Xth edition, respectively.
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2.
Sylwia Smarzewska Sławomira Skrzypek Barbara Bachowska Piotr Bałczewski Witold Ciesielski 《Central European Journal of Chemistry》2011,9(5):840-845
Electrochemical oxidation of methylthiomethyleneisoquinolinium chloride (MTMIQ), the first alkylthiomethyl substituted ammonium
salt, which is fully miscible with water has been investigated by voltammetric (SWV) method using glassy carbon electrode.
On the electrode, MTMIQ undergoes oxidation at the potential near Ep = 0.07V (vs. Ag/AgCl/3 M KCl). The influence of the pH
of buffers, amplitude, frequency, step potential on the received signal was studied. The best results were obtained with a
citrate buffer at a pH of 5. The oxidation peak current used for MTMIQ voltammetric determination was in the range of 2–8×10−5 mol L−1, LOD = 3.7×10−6, LOQ = 1.2×10−5. The product of the oxidation was accumulated at the working electrode and was investigated by spectroscopic method. Mechanistic
pathways of the oxidation have been proposed.
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3.
Jaromíra Chýlková Renáta Šelešovská-Fadrná Jaroslava Machalíková 《Central European Journal of Chemistry》2007,5(2):479-495
The optimal process of pre-treatment and activation of gold rotating disc electrode (AuRDE) before voltammetric determination
of mercury is proposed. This treatment encompasses polishing of the electrode surface, electrochemical cycling, and activation.
This procedure both increases determination sensitivity as well as improves determination reproducibility. The detection limit
on the working electrode achieved using this approach amounted to 8.26·10−10 mol L−1for direct mercury determination in water solution (applying 200 s running accumulation). The procedure of the quantitative
mercury isolation from complicated sample matrix was developed as well. It provides better selectivity and significant increase
of sensitivity of mercury determination. In case of mercury isolation from one liter of water the detection limit is 6.23·10−11 mol L−1 (analyzing a greater sample volume the determined concentration could be lower).
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4.
Violeta D. Mitic Snezana D. Nikolic Vesna P. Stankov-Jovanovic 《Central European Journal of Chemistry》2010,8(3):559-565
A kinetic spectrophotometric method for hydrazine determination in the range of 9.36×10−7 to 4.37×10−5 mol dm−3, based on the inhibitory effect of hydrazine on the oxidation of Victoria Blue 4- R by KBrO3, was developed and validated. Kinetic parameters are reported for both the indicating and the inhibiting reaction. The detection
limit was established as 9.98×10−8 mol dm−3. The selectivity of the proposed method was tested considering the influence of different ions that may be present in real
samples. The method was successfully applied for hydrazine determination in various samples (very pure water from the water-steam
system of a power plant and Isoniazid tablets, a pharmaceutical product).
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5.
Ibuprofen membrane electrodes based on different plasticizers: diisobutyl phthalate (DIBP), o-nitrophenyloctyl ether (o-NPOE),
dioctyl sebacate (DOS) and tetraoctylammonium 2-(4-isobutylphenyl)propionate were prepared. All electrodes show: a near Nernstian
slope of characteristic (58.3–60.9 mV decade−1) in the measurement range (10−4–10−1 mol L−1), limit of detection (5.0×10−5 mol L−1), really long lifetime (12 months), dependence of the electrode potential on pH (5.5–9.0), reproducibility of potential (0.6–1.2
mV) and selectivity coefficients in relation to some organic and inorganic anions. The electrodes were applied for the determination
of ibuprofen in tablets by the calibration curve method and the standard addition method.
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6.
Joanna Lenik Cecylia Wardak Barbara Marczewska 《Central European Journal of Chemistry》2008,6(4):513-519
Naproxen membrane electrodes based on different plasticizers and the quaternary ammonium salts (QASs) dimethyldidecylammonium
bromide, methyltrioctylammonium chloride, or tetraoctylammonium chloride, were prepared. The following basic parameters were
investigated for the optimal electrode: measurement range (10−4 − 10−1 mol L−1), slope of the linear range of the calibration curve (−58.3 mV decade−1), limit of detection (6.0 × 10−5 mol L−1), lifetime (2.5 months), dependence of the electrode potential on pH (5.5 − 9.0), reproducibility of potential (1.2 mV) and
selectivity coefficients in relation to selected organic and inorganic anions. The electrode was utilized for determination
of naproxen in tablets by the calibration curve method and the standard addition method.
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7.
The construction and optimization of five new types of miniaturized flow-through electrolytic cells with lead cathode and
platinum anode for electrochemical hydride generation in atomic absorption spectrometry (HG-QFAAS) were achieved during this
research study. The ion-exchange membrane was not part of these cells and only one carrying electrolyte for both electrode
chambers was used. Hydride generation efficiency achieved was either comparable or higher than the one recorded for the classic
thin-layer generation cell. The inner volume of the cathode chamber was reduced to a quarter of the classic thin-layer flow-through
cell. Compared to the commonly used thin-layer flow-through cell, higher sensitivity (7.32×103 dm3 μg−1) and better limit of detection (0.32 μg dm−3) were obtained for selenium determination using two of these new generators.
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8.
Morteza Bahram Khalil Farhadi Farzin Arjmand 《Central European Journal of Chemistry》2009,7(3):524-531
A new differential pulse voltammetric method for dopamine determination at a bare glassy carbon electrode has been developed.
Dopamine, ascorbic acid (AA) and uric acid (UA) usually coexist in physiological samples. Because AA and UA can be oxidized
at potentials close to that of DA it is difficult to determine dopamine electrochemically, although resolution can be achieved
using modified electrodes. Additionally, oxidized dopamine mediates AA oxidation and the electrode surface can be easily fouled
by the AA oxidation product. In this work a chemometrics strategy, partial least squares (PLS) regression, has been applied
to determine dopamine in the presence of AA and UA without electrode modification. The method is based on the electrooxidation
of dopamine at a glassy carbon electrode in pH 7 phosphate buffer. The dopamine calibration curve was linear over the range
of 1–313 μM and the limit of detection was 0.25 μM. The relative standard error (RSE %) was 5.28%. The method has been successfully
applied to the measurement of dopamine in human plasma and urine.
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9.
Cecylia Wardak 《Central European Journal of Chemistry》2008,6(4):607-612
A new all plastic sensor for Co2+ ions based on 2-amino-5 (hydroxynaphtyloazo-1′)-1,3,4 thiadiazole (ATIDAN) as ionophore was prepared. The electrode exhibits
a low detection limit of 1.5 × 10−6 mol L−1 and almost theoretical Nernstian slope in the activity range 4.0 × 10−6–1 × 10−1 mol L−1 of cobalt ions. The response time of the sensor is less than 10 s and it can be used over a period of 6 months without any
measurable divergence in potential. The proposed sensor shows a fairly good selectivity for Co(II) over other metal ions.
The electrode was successfully applied for determination of Co2+ in real samples and as an indicator electrode in potentiometric titration of Co2+ ions with EDTA.
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10.
Azza A. Shoukry Mohamed M. Shoukry Mohamed N. Hafez 《Central European Journal of Chemistry》2010,8(4):797-805
The kinetics of base hydrolysis of glycine, histidine, and methionine methyl esters in the presence of [Pd(pip)(H2O)2]2+ complex, where pip is piperazine, is studied in aqueous solutions, at T = 25°C, and I = 0.1 mol dm−3. The rate of ester hydrolysis for glycine methyl ester is studied at different temperature and dioxane/water solutions of
different compositions. The kinetic data are fit under the assumption that the hydrolysis proceeds in one step. The activation
parameters for the base hydrolysis of the complexes are evaluated
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11.
Jinzhang Gao Yingying Zhang Jie Ren Ming Li Wu Yang 《Central European Journal of Chemistry》2010,8(3):602-606
A sensitive and convenient method for the determination of trace europium ions using an oscillating chemical reaction involving
Ce(IV) - KBrO3 - acetone - oxalic acid - H2SO4 was proposed. The results indicated that the changes in oscillating period (T) was linearly proportional to the negative
logarithmic concentration of Eu3+ (-log C) in the range of 1.41 × 10−8 ˜ 1.41 × 10−4 mol L−1 (r = 0.9982) with a detection limit of 1.04 × 10−9 mol L−1. The recoveries were limited to the range of 99.5% to 100.8%. Under the same conditions, other rare earth ions did not interfere
with the determination of Eu3+. In addition, a perturbation mechanism was also discussed briefly.
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12.
Hana Dejmkova Candan Dag Jiri Barek Jiri Zima 《Central European Journal of Chemistry》2012,10(4):1310-1317
New methods for the determination of metoclopramide, antiemetic and gastroprokinetic pharmaceutical, were developed, using
differential pulse voltammetry (DPV) and flow injection analysis (FIA) with amperometric detection on a boron-doped diamond
film electrode. Electrode pretreatment necessary to ensure the stable results was investigated and it was found, that while
DPV requires frequent electrode cleaning, FIA with a sufficiently high flow rate can maintain a stable signal with no signs
of electrode passivation. The calculated quantification limits of the DPV and FIA with amperometric detection were 0.13 μmol
L−1 and 0.015 mmol L−1, respectively. The applicability of the new methods was verified by the determination of metoclopramide in a pharmaceutical
preparation. FIA with amperometic detection proved to be sensitive, accurate and, due to the resistance of the electrode to
the passivation, also simple to handle.
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13.
Grzegorz Lota Krzysztof Fic Krzysztof Jurewicz Elzbieta Frackowiak 《Central European Journal of Chemistry》2011,9(1):20-24
Electrochemical storage of hydrogen in activated carbon material has been investigated using different parameters of cathodic
polarization. It has been proven that application of short galvanostatic pulses could be efficient for hydrogen storage in
microporous carbon material. Charging current loads from 50 mA g−1 to 32 A g−1 have been used showing correlation between hydrogen capacity, time of charging and electrical efficiency. The anodic charge
equivalent to electrooxidation of 1.0 wt% of hydrogen can be already reached after 90 s of cathodic polarization. Temperature
effect has been also evaluated and a gradual increase of hydrogen capacity with a better pronounced oxidation plateau was
obtained at higher temperatures. Reversible electrosorption of hydrogen is a useful reaction in supercapacitor performance
and it might have a potential application for a negative electrode of supercapacitor as well as reversibly operating electrode
in the secondary cell.
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14.
Zholt Kormosh Iryna Hunka Yaroslav Bazel Andriy Laganovsky Iryna Mazurenko Nataliya Kormosh 《Central European Journal of Chemistry》2007,5(3):813-823
The potentiometric response characteristics of a diclofenac selective electrode, based on ion association in different plasticizers,
were compared. The sensitivity, working range, detection limit and selectivity of membrane sensors demonstrated significant
dependence on the type of plasticizers. The potentiometric unit presented a linear response toward diclofenac concentrations
between 1 × 10−5 − 5 × 10−2 mol L−1, with slopes of approximately 60 mV dec−1, and exhibited a response time of 3 s. The potentiometric analysis of sodium diclofenac in pharmaceutical formulations was
perfomed by the membrane electrode proposed and compared with the results of potentiometric titration given by the Pharmacopoeia
of Ukraine.
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15.
Jinzhang Gao Jing Liu Jie Ren Xiuli Niu Yingying Zhang Wu Yang 《Central European Journal of Chemistry》2009,7(3):298-302
This paper described the determination of p-nitroaniline in a double organic substrate oscillating system of tartrate-acetone-Mn2+-KBrO3-H2SO4. Under the optimum conditions, temperature was chosen as a control parameter to design the bifurcation point and proposed
a convenient method for determination of p-nitroaniline. Results showed that the system consisting of 3.5 mL 0.06 mol L−1 tartrate, 4.0 mL 0.7 mol L−1 H2SO4, 1.5 mL 1.5×10−4 mol L−1 MnSO4, 4.0 mL 0.4 mol L−1 acetone and 7.0 mL 0.05 mol L−1 KBrO3 was very sensitive to the surrounding at 33.5°C. A good linear relationship between the potential difference and the negative
logarithm concentration of p-nitroaniline was obtained to be in the range of 2.50×10−7∼3.75×10−5 mol L−1 with a lower detection limit of 2.50×10−8 mol L−1.
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16.
Mónica Díaz-Pérez Manuel Aboal-Somoza Pilar Bermejo-Barrera Adela Bermejo-Barrera 《Central European Journal of Chemistry》2008,6(4):520-525
Preliminary results of development of a direct and fast method of determination of antimony in samples of tap water using
GFAAS are presented. The found levels of antimony were lower than permitted for human consumption. A mixture of Pd and Mg(NO3)2 (concentrations in the injected solution: 8.6 μg mL−1 and 5.8 μg mL−1 respectively) was used as the chemical modifier. The pyrolysis and atomization temperatures were 1000 and 1700°C, respectively
and the mean analytical recovery 98.2%.
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17.
Titania layers obtained by a sol-gel technique doped with redox mediator, Meldola’s Blue, were employed for construction of
a new NADH senor. Optimization of preparation process as well as experimental conditions affecting the response of the sensor
were examined. Under optimal conditions NADH could be determined in the wide linear range from 90 to 2300 μM with detection
limit 12 μM and a high sensitivity 12.5 nA μM−1. The usefulness of developed sensor was preliminarily checked in determination of NADH forming during enzymatic oxidation
of ethanol catalyzed by alcohol dehydrogenase (ADH).
相似文献
18.
Yuxi Ren Zhen Chen Riyao Chen Xi Zheng Yamin Geng 《Central European Journal of Chemistry》2007,5(1):177-190
The preparation of SAMS-CMC-CS bipolar membrane grafted onto CMC by SAMS was reported. The cross-section view of SAMS-CMC-CS
BM were studied by SEM. FT-IR spectrum indicated that SAMS-CMC-CS BM contained-SO
3
−
,-COO− and −N=CHR functional groups. Compared with CMC-CS BM, SAMS-CMC-CS BM appears to have better mechanical strength and chemical
stability in alkali solution at [OH−]≥9.5 mol/L, with a swelling of 55 %. The electrochemical properties of SAMS-CMC-CS BM were also studied. SAMS-CS-CMC BM not
only effectively prevented FeO
4
2−
from diffusing into the cathode chamber, but also played an important role in the supply of OH− consumed during the electro-generated FeO
4
2−
process.
相似文献
19.
Dmitriy A. Golovko Virender K. Sharma Olga. V. Pavlova Elena. A. Belyanovskaya Igor. D. Golovko Victoria. I. Suprunovich Radek Zboril 《Central European Journal of Chemistry》2011,9(5):808-812
A new amperometric titration method was developed for quantitative determination of ferrate(VI) (FeVIO4
2−) in the 7.06×10−5−5.73×10−3 M concentration range. Chromium(III) hydroxide solution was used as the titrant. The diffusion current (Id) had a linear
relationship with the concentration of ferrate(VI) and slopes were dependent on the concentration of NaOH. The amperometric
titration could detect a lower concentration of ferrate(VI) than could potentiometric and colorimetric titrations. The method
was applied successfully to determine concentrations of ferrate(VI), generated electrochemically, in strong alkaline solutions.
相似文献
20.
The present work reports the synthesis, characterization and performance of a new zinc(II) complex of [Zn(C3H7-bim)2Br2] (bim = benzimidazole) as electrocatalyst for trichloroacetic acid and bromate reduction. Its structure was characterized
by X-ray crystallography, IR spectroscopy and elemental analysis. The zinc atom adopts a distorted tetrahedral geometry by
coordinating to two bromine atoms and two nitrogen atoms from two 1-propyl-1H-benzo[d]imidazole ligands. The electrochemical behavior and electrocatalysis of the zinc complex bulk-modified carbon paste electrode
(Zn-CPE) have been studied by cyclic voltammetry. The Zn-CPE shows good electrocatalytic activities toward the reduction of
trichloroacetic acid and bromate. The detection limit and the sensitivity are 0.05 μM, 67.43 μA μM−1 for trichloroacetic acid detection, and 0.02 μM, 69.94 μA μM−1 for bromate detection, respectively. This modified electrode shows good reproducibility, high stability, low detection limit,
technical simplicity and possibility of rapid preparation, which is important for practical applications.
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