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PubMedDate not supplied

Voltammetric determination of montelukast sodium in dosage forms and human plasma.

The voltammetric behaviour of montelukast (MKST) was studied using cyclic voltammetry, direct current (DCt), differential pulse polarography (DPP) and alternating current (ACt) polarography. MKST exhibited well-defined cathodic waves over the range pH range 1-5. No anodic waves were produced over the same pH range. At pH 1, the analytical pH; the diffusion current constant (Id) was 2.2+/-0.01 microA l mmol-1. The current concentration plot was rectilinear over the range 2-20 microg ml-1 with correlation coefficient (n=10) of 0.9943. The lower limit of detection (S/N=2) was 0.2 microg ml-1 (3.41x10(-7) M). The wave has been characterised as being diffusion-controlled, although adsorption phenomenon played a limited role in the electrode reaction. The proposed method was successfully applied to the determination of MKST in commercial tablets, and results were in agreement with those given with a reference HPLC method. The method was further extended to the in vitro determination of the drug in spiked human plasma. The mean % recovery (n=5) was 101.38+/-3.85. The number of electrons transferred in the reduction process could be accomplished and a proposal of the electrode reaction was proposed.

Acetates↗

PubMed2004

Polarographic behaviour of Aceclofenac, Tenoxicam and Droxicam in a methanol-water mixture.

A polarographic study about how three anti-inflammatories, such as Aceclofenac, Tenoxicam and Droxicam behave, using tast polarography (TP) and differential pulse polarography (DPP) was carried out. These studies were always carried out in a media formed by Methanol-Britton-Robinson aqueous buffer (0.1M) (4:96 (v/v)) due to the low solubility of these drugs in water. A strong influence of pH on analytical signals was observed, showing that the optimal pH values were between 4 and 5. Using DPP in the optimal experimental conditions, a detection limit of 10 ppb for Tenoxicam and Droxicam and 52 ppb for Aceclofenac was reached. The DPP proposed method was successfully applied to the determination of the active compounds in commercial drugs.

Anti-Inflammatory Agents, Non-Steroidal↗

PubMed2005

Electrochemical study of imipenem's primary metabolite at the mercury electrode. Voltammetric determination in urine.

Imipenem shows a fast chemical conversion to the more stable imin form (identical to that from biochemical dehydropeptidase degradation) in aqueous solutions that shows a wave at lower cathodic potential than the imipenem one. The aim of this work is the study of the electrochemical behaviour of the primary metabolite of imipenem (M1) and the proposal of electrochemical methods for the determination of M1 in human urine samples. Electrochemical studies were realized in phosphate buffer solutions over pH range 2.0-8.0 using differential pulse polarography, dc-tast polarography, cyclic voltammetry and linear sweep voltammetry (staircase). In acidic media, a non-reversible diffusion-controlled reduction involving two electrons and two protons occurs and the mechanism for the reduction was suggested. A differential pulse polarographic method for the determination of M1 in the concentration range 10(-6) to 10(-4)M with a detection limit of 4.5 x 10(-7)M was proposed. Also, a method based on controlled adsorptive pre-concentration of M1 on the hanging mercury drop electrode (HMDE) followed by linear sweep voltammetry allows its determination in the concentration range 2 x 10(-9) to 4 x 10(-8)M with a detection limit of 1.05 x 10(-9)M. The proposed methods have been used for the direct determination of M1 in spiked human urine and real human-derived urine with good results and should be appropriate for monitoring purposes.

Biotransformation↗

PubMed2006

Voltammetric assay of the anthelmintic veterinary drug nitroxynil in bulk form and formulation at a mercury electrode.

The electrochemical behavior of the anthelmintic veterinary drug nitroxynil at the mercury electrode was studied in a series of Britton-Robinson universal buffer of pH 1.9-11 containing 20% (v/v) ethanol using dc-polarography cyclic voltammetry and controlled-potential coulometry. The voltammograms exhibited two irreversible cathodic steps over the pH range 1.9-10.2; the height of the first step is double that of the second one. Controlled-potential coulometry in the B-R universal buffer of pH 1.9-10 at a mercury pool working electrode revealed the consumption of four and two electrons via the first and second reduction steps, respectively, which attributed to reduction of the NO2 group to the hydroxylamine stage (first step), and then to the amine stage (second step). Three voltammetric analytical procedures including dc-polarography, differential-pulse adsorptive stripping voltammetry and square-wave adsorptive stripping voltammetry were optimized for the direct determination of bulk nitroxynil. The three proposed procedures were applied for analysis of bulk nitroxynil with limits of detection of 3 x 10(-5), 1.31 x 10(-8) and 8.4 x 10(-10)M and limits of quantification of 1 x 10(-5), 4.36 x 10(-8) and 2.80 x 10(-9)M, respectively. The three procedures were successfully applied to the determination of nitroxynil in formulation (Dovenix, 25% nitroxynil injection solution) without the necessity for sample pretreatment and/or time-consuming extraction steps prior to the analysis.

Antiplatyhelmintic Agents↗

PubMed1998

Pulse polarographic (constant and increasing) determinations of doxazosin in pharmaceutical tablets.

The optimum conditions using DC polarography and the determination of doxazosin employing SIAP and SCAP polarographic techniques are described in this study. All the experiments were conducted in the supporting electrolyte consisting of 20% ethanol (v/v), 0.2 M KCl and 0.2 M acetate buffer at various pH values in order to examine the optimum conditions, and pH 3.5 for the determination of doxazosin. Well-defined curves were obtained in the pH range of 1.5-7.5. The system was diffusional and irreversible at pH 3.5. The calibration studies were performed by using SIAP and SCAP polarography and satisfactory results were observed for all techniques. Since the sensitivity of SIAP and SCAP techniques were higher than the others, the determination of doxazosin was performed in filtered and unfiltered tablet solutions containing 4 mg active material. In the analysis of a tablet, the relative standard deviations (Srel %) of the techniques are in the filtered solutions +/- 0.9 (SIAP), +/- 0.8 (SCAP) and in the unfiltered solutions +/- 0.7 (SIAP), +/- 0.8 (SCAP) and no interference was observed during the analysis. The determination methods proposed in this study appear to be accurate, rapid and practicable. Therefore, these techniques may be suitable for the content uniformity tests.

Antihypertensive Agents↗

PubMed1999

Electrochemical study on the determination of tinidazole in tablets.

The electrochemical reduction of tinidazole has been carried out in aqueous solution in the pH range 1.8-11.3 by differential-pulse (DP) polarography. Tinidazole exhibits one or two reduction peaks depending on pH. In strongly acidic solution (pH < 4.5), one reduction peak was obtained and it was suitable for analytical purposes. A method for the determination of tinidazole by DP polarography in Britton-Robinson buffer of pH 3.0, which allows quantification over the range 0.03-7.30 microg/ml, was proposed. The method was successfully applied to the determination of tinidazole in tablets with mean recovery and relative standard deviation of 98.7 and 3%, respectively. Excipients did not interfere in the determination.

Antitrichomonal Agents↗

PubMed2003

[Sonografic evaluation of oxygenation in head and neck cancer].

BACKGROUND: Tumor oxygenation is an important aspect of radiosensitivity. The authors describe a new method for a non-invasive assessment of tumor oxygenation in head and neck cancer. PATIENTS AND METHODS: A group of 20 patients with neck metastases of squamous cell cancer of the head and neck region was surveyed. At first a pO (2)-polarography was performed in the metastatic cervical nodes to investigate the tissue oxygenation. In a second step, the vascularisation of these nodes was visualised by color duplex sonography. In order to evaluate the extent of vascularisation in these nodes, the density of color pixels was quantified by a custom-made software program. The color pixel density and the pO (2) values were correlated and the statistic significance was calculated by Pearson's test. RESULTS: The mean vascularisation as evaluated by the means of color duplex sonography was 7.78 % [95 % CI 6.04 - 9.51]. The interindividual pO (2) values in the stroma of metastatic lymph nodes ranged between 9.0 and 27.4 mmHg (16.6 [95 % CI 14.06 - 19.13]). The mean values of pO (2)-fractions < 2.5/< 5.0/10 mm Hg were 32.25 %, 44.25 % and 53.29 % respectively. The median value of the pO (2)-fraction was 10.49 % [95 % CI 7.13 - 13.85]. The vascularisation as evaluated by color pixel density showed a statistically significant correlation with the pO (2)-fractions < 5.0 and < 10 mmHg (p < 0.045 and < 0.0001) and with the mean (p < 0.002) and median values of tissue pO (2) values (p < 0.0001) in polarography. CONCLUSION: The results in a limited number of patients suggest, that the proposed sonographic method allows a reliable non-invasive evaluation of tissue oxygenation in cervical metastases of squamous cell head and neck cancers.

Adult↗

PubMed1983

Polarographic determination of butorphanol tartrate.

A new indirect polarographic method is proposed for the determination of butorphanol tartrate in the injectable solution form (Stadol). Direct-current polarography and differential pulse polarography (DPP) were applied for the study of authentic butorphanol and its injectable solution form in alkaline medium after nitration with 1 M potassium nitrite in presence of 1 M hydrochloric acid. The standard addition method was employed for the evaluation of the results and the mean percentage found for the injectable solution form was 99.2 +/- 1.0.

Butorphanol↗

PubMed1995

Stability constants of Zn(II), Pb(II), Cd(II) and Cu(II) complexes with hematoxylin.

The composition and stability constants of the complexes of Zn(II), Pb(II), Cd(II) and Cu(II) with hematoxylin have been studied using direct current polarography and differential pulse polarography. The results showed the formation of 1:2 (M:L) complexes for Zn(II) and Pb(II), and a 1:6 (M:L) complex for Cd(II). However, the formation of copper-hematoxylin complex is irreversible. The values of the formation constants for the above complexes at 298, 308 and 318K were calculated as well as the relevant thermodynamic parameters.

Cadmium↗

PubMed2002

Differential pulse polarographic determination of uranium(VI) in complex materials after adsorption of its trifluoroethylxanthate cetyltrimethylammonium ion-associated complex on naphthalene adsorbent.

Uranium(VI) is adsorbed as a uranium trifluoroethylxanthate (TFEX)-cetyltrimethylammonium (CTMA) ion-pair complex on microcrystalline naphthalene quantitatively in the pH range 4.2 - 7.0. Without cetyltrimethylammonium as the counter ion, the adsorption is hardly 70%. The metal has been desorbed with HCI and determined with a differential pulse polarograph. Uranium can alternatively be quantitatively adsorbed on TFEX-CTMA-naphthalene adsorbent packed in a column at a flow rate of 1 - 5 ml/min and determined similarly. A well-defined peak has been obtained in this medium at -0.20 V versus a saturated calomel electrode. Cyclic voltammetry, differential pulse polarography and D.C. polarography studies indicate that uranium has been reduced irreversibly under these conditions. The detection limit is 0.30 microg/ml at the minimum instrumental settings (signal-to-noise ratio of 2) (with a preconcentration factor of 10, the detection limit would be 30 ng/ml for uranium when the volume in the cell is 15 ml). However if the volume in the cell is 5 ml, it would have been 10 ng/ml with a preconcentration factor of 30. Linearity is maintained in a concentration range of 0.5 - 19.0 microg/ml (2.1 - 79.83 x 10(-9) M) with a correlation factor of 0.9994 and a relative standard deviation of +/-1.1% (in this case 7.5 microg may be concentrated from 150 ml of the aqueous sample where its concentration is as low as 50 ng/ml). Various parameters, such as the effect of the pH, volume of the aqueous phase, flow rate and the interference of a large number of metal ions and anions on the determination of uranium, have been studied in detail to optimize the conditions for its trace determination in various complex materials, like alloys, coal fly ash, biological, synthetic, and waste-water samples.

Adsorption↗

PubMedDate not supplied

Differential pulse polarographic determination of procymidone in formulations and wine.

The dicarboximide fungicide procymidone was studied systematically by using direct current polarography, cyclic voltammetry, differential pulse polarography (DPP), controlled potential electrolysis, and millicoulometry in the universal buffer medium with dimethylformamide as the solvent. Procymidone exhibited a single well-defined polarographic wave in the pH range 2.0-6.0, leading to the formation of the hydroxy compound. The overall reduction process was diffusion-controlled and adsorption-free. The variation of half-wave potential with pH, the concentration of the analyte, and other experimental conditions are described. The reduction mechanism proposed is an overall 4-electron process, in which the dicarboximide group is reduced. DPP was used to determine procymidone in agricultural formulations and wine at the optimum conditions found; a detection limit of 2.4 x 10(-9) M was estimated. The results obtained by the proposed method were also compared with those obtained by other methods.

Bridged Bicyclo Compounds↗

PubMed1976

Determination of arsenic and selenium in foods by electroanalytical techniques.

Arsenic and selsnium are determined in foods be differential pulse polarography and cathodic stripping voltammetry. The sample is digested with nitric acid and magnesium nitrate and then dissolved in dilute hydrochloric acid. An aliquot is removed, the arsenic is chemically reduced to the trivalent state, and interferences are removed by ion exchange before polarography. Selenium is determined in a second aliquot by cathodic stripping voltammetry. Recoveries for both elements in several foods were from 90 to 110%. The relative standard deviations for arsenic at 5 ppm and selenium at 0.48 ppm were 5.8 and 7.3%, respectively.

Arsenic↗

PubMed2003

Physico-chemical properties and spectrophotometric determination of biologically active 1-alkyl-2-(2-pyridyl)pyridinium bromides.

Physico-chemical properties of compounds prepared from 2,2'-bipyridine, 1-alkyl-2-(2-pyridyl)pyridinium bromides, were investigated by DC polarography and by GC-MS. Their ionization potentials were calculated. Additionally, the formation of associates with bromothymol blue and methyl orange during the spectrophotometric determination was measured. It was determined that 1-alkyl-2-(2-pyridyl)pyridinium ions are reduced by 2 one-electron steps in a DC polarography system. The reduction potentials are not related to the ionization potential values calculated for the substances investigated. The carcinogenic potential (tg alpha) of the parent compound 2,2'-bipyridine and of a series of 1-alkyl derivatives was very low indicating that the compounds are not carcinogenic. The MS fragmentation patterns indicate the low stability of the 1-alkyl substituents. It was shown that 2,2'-bipyridine is either fragmented to two pyridine ions or the--N=CH--fragments are removed. Additionally, spectrophotometric determinations of colored associates of 1-alkyl-2-(2-pyridyl)pyridinium bromides with bromothymol blue and methyl orange were investigated and the optimal condiditions for these determinations are reported.

2,2'-Dipyridyl↗

PubMedDate not supplied

Voltammetric behavior of zaleplon and its differential pulse polarographic determination in capsules.

In this work both the electrochemical behavior and the analysis of the hypnotic pyrazolopyrimidine derivative zaleplon were studied. Zaleplon in ethanol-0.1M Britton Robinson buffer solution (30-70) showed 2 irreversible, well-defined cathodic responses in the pH range of 2-12 using differential pulse polarography (DPP), tast polarography, and cyclic voltammetry. From chronocoulometric studies, it was possible to conclude that one electron was transferred in each reduction peak or wave. For analytical purposes, the DPP technique working at pH 4.5 for peak I was selected, which exhibited adequate repeatability, reproducibility, and selectivity. The recovery was 99.97 +/- 1.52%, and the detection and quantitation limits were 5.13 x 10(-7)M and 1.11 x 10(-6)M, respectively. The DPP method was applied successfully to the individual assay of capsules in order to verify the content uniformity of zaleplon. Treatment of the sample is not required because the excipients do not interfere, the method is not time consuming, and it is less expensive than column liquid chromatography.

Acetamides↗

PubMed2006

Electrochemical behavior and determination of tumor inhibiting or promoting activities of flavonoids.

This paper deals with determination of the tumor inhibiting or promoting activities of 11 flavonoids performed by DC polarography. Flavonoids were tested in the presence of polyaromatic carcinogen 7,12-dimethylbenz(a)anthracene (DMBA) or in combination with DMBA and 12-O-tetradecanoylphorbol-13-acetate (TPA), which is known as a specific tumor promoter for epidermal carcinogenesis. We found that in this experimental system the promotory or inhibitory activities of studied flavonoids depend on the number and position of hydroxyl groups in their chemical structures and are related to the polarographic behavior of these compounds. Flavonoids, which are hydroxylated at the ring B, are reduced in anhydrous DMF on a mercury dropping electrode in two one-electron steps. Absence of the hydroxyl groups in these positions caused their reduction in three one-electron steps. Similarly, flavonoids with hydroxyl groups at the ring B have been shown to inhibit the activities of DMBA (2.7-45.9%) and of DMBA + TPA (47.2-78.2%). Missing hydroxyl groups caused weaker inhibitory activity against DMBA + TPA (19.01-38.74%) and the enhancement of DMBA activity (31.08-66.21%). Presented data demonstrated that the electrochemical method--DC polarography is very sensitive, simple technique for determination of the tumor inhibiting or promoting activities of the studied compounds.

9,10-Dimethyl-1,2-benzanthracene↗

PubMed1985

Voltammetry of tobacco mosaic virus and its isolated protein at the graphite electrode.

The electrochemical behaviour of tobacco mosaic virus (TMV) and its isolated protein was studied using differential pulse (DP) voltammetry at a graphite electrode and by direct current (DC) polarography in Brdicka solution. TMV and its isolated protein were found to be electrooxidized at the graphite electrode in the adsorbed state. Both species yielded two oxidation peaks on DP voltammograms. The first, more negative peak, corresponded to electrooxidation of tyrosine residues, whereas the other, more positive, peak corresponded to electrooxidation of tryptophan residues. DC polarography was used to detect degradation of TMV and denaturation of TMV-protein induced by an increased pH and by the addition of urea, respectively. These structural transformations resulted in increased DP voltammetric oxidation currents as recorded using a graphite working electrode. It has been suggested that the higher oxidation currents were due to an increase in the number of tyrosine and tryptophan residues accessible to the reaction at the graphite electrode. The results of these electrochemical investigations were in a good agreement with the estimation of the accessibility of tyrosine and tryptophan residues based on the well-explored three-dimensional structure of TMV and its isolated protein.

Electric Conductivity↗

PubMed1985

Method for the preparation of plasmid DNA suitable for physicochemical measurements.

A method has been developed for the isolation of plasmid DNA suitable for physical and physicochemical measurements. The procedure is based on the deproteinization of the cleared lysate of bacterial cells (after amplification of plasmids by chloramphenicol) by phenol at pH 8.0 and subsequent removal of chromosomal DNA by means of phenol at pH 4.0 and separation of RNA on a hydroxyapatite column at higher temperature. ColE1 DNA sample was compared with samples of the same DNA prepared by three thus far used methods. Samples obtained by means of the latter methods were contaminated with chromosomal DNA, RNA, or ethidium bromide. The presence of ethidium bromide in the DNA sample was a factor interfering in the electrochemical analysis, chromosomal DNA and RNA were disturbing in the use of other methods. DNA separated by the method devised by us was free of any detectable contaminants and fulfilled the high requirements for sample purity of differential pulse polarography. Measurements performed by means of differential pulse polarography showed that the content of single-stranded segments in superhelical ColE1 DNA is less than 0.15% (i.e. less than 20 bases per molecule). This is in keeping with the notion that a cruciform is formed in this DNA (as a result of tension due to supercoiling) in the region of inverted repeat sequence, containing only 5 bases in the single-stranded loop region.

Animals↗

PubMed1979

Complexes of technetium with pyrophosphate, etidronate, and medronate.

The reduction of [99Tc]pertechnetate was studied as a function of pH in complexing media of pyrophosphate, methylene diphosphonate (MDP), and ethane-1, hydroxy-1, and 1-diphosphonate (HEDP). Tast (sampled d-c) and normal-pulse polarography were used to study the reduction of pertechnetate, and normal-pulse polarography (sweeping in the anodic direction) to study the reoxidation of the products. Below pH 6 TcO4-was reduced to Tc(III), which could be reoxidized to Tc(IV). Above pH 10, TcO4-was reduced in two steps to Tc(V) and Tc(IV), each of which could be reoxidized to TcO4-. Between pH 6 and 10 the results differed according to the ligand present. In pyrophosphate and MDP, TcO4- was reduced in two steps to Tc(IV) and Tc(III); Tc(III) could be reoxidized in two steps to Tc(IV) and TcO4-. In HEDP, on the other hand, TcO4- was reduced in two steps to Tc(V) and Tc(III), and could be reoxidized to Tc(IV) and TcO4-. Additional waves were observed; they apparently led to unstable products.

Diphosphates↗