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Voltammetric determination of some alkaloids and other compounds in pharmaceuticals and urine using an electrochemically activated glassy carbon electrode

100%
Câmpean A., Tertiş M., Săndulescu R.
Open Chemistry
|
2011
|
vol. 9
|
issue 4
688-700
EN
Electrochemical behaviour of some alkaloids, namely: caffeine, aminophylline, theophylline, codeine phosphate and papaverine hydrochloride, that are in solution in various combinations or in the presence of other compounds contained in pharmaceuticals or in real samples (urine) was investigated using cyclic voltammetry (CV), square-wave voltammetry (SWV) and differential pulse voltammetry (DPV) on electrochemically activated glassy carbon electrode. [...] The proposed electroanalytical methods were successfully applied in the simultaneous determination of these alkaloids in different combination or in the presence of other compounds. The great part of these combinations can be analyzed simultaneously because they practically do not interfere. The electrochemical test methods attempted to detect the presence of alkaloids in urine samples collected from subjects who consumed coffee (caffeine), and from a patient under treatment with Miofilin® (aminophylline). Urine samples were determined after filtration, without prior dilution and after dilutiion with acetate buffer at pH 4.5. Best results were obtained using DPV performed on electrochemically activated glassy carbon electrode. Thus in samples taken from subjects who drink coffee the caffeine concentration detected was 6.21×10−7 mol L−1 in the first sample and 7.77×10−7 mol L−1 in the second sample, while aminophylline concentration detected was 1.15×10−7 mol L−1.
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Method validation in quantitative electrochemical analysis of colchicine using glassy carbon electrode

100%
Bodoki E., Săndulescu R., Roman L.
Open Chemistry
|
2007
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vol. 5
|
issue 3
766-778
EN
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. [...]
3
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Electrochemical behavior of some purine derivatives on carbon based electrodes

100%
Câmpean A., Tertiş M., Săndulescu R.
Open Chemistry
|
2011
|
vol. 9
|
issue 3
466-473
EN
The electrochemical behaviour of three purine derivatives was investigated by cyclic voltammetry on different electrode materials: glassy carbon in native form and electrochemically activated, carbon paste electrode unmodified or modified with 1, 4-benzoquinone. The preliminary study obtained on solid electrodes was extended to graphite based planar screen-printed electrodes, unmodified and modified with multi-wall carbon nanotubes, or cobalt phthalocyanine. The influence of some experimental parameters (pH, scan rate, concentration and electrolytic medium) on the electrochemical behaviour of these alkaloids was also examined. The electrochemical oxidation of purine derivatives is an irreversible and diffusion controlled process, proved by the linear dependence between the peak potentials and the logarithm of scan rates and between the anodic peak current and the square root of scan rate.
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