Differential-pulse polarography of amino acids in acetaldehyde-borax medium

A differential-pulse polarographic method for the determination of amino acids is reported, based on the formation of Schiff's base compounds in borax buffer solution (pH 10.10) containing acetaldehyde. The compounds are reduced at a mercury electrode with peak potentials of about ?1.5 V (vs. SCE) and well defined polarographic waves are obtained which can be used to determine amino acids in borax medium. The differential-pulse polarographic method was found to be the most sensitive and suitable for the determination of amino acids in the concentration range 1 × 10^?6–8 × 10^?4 M (lysine) and 2.8 × 10^?6–1 × 10^?3 M (arginine). The polarographic characteristics of these waves were studied by differential-pulse polarographic and cyclic voltammetric methods. The waves are ascribed to the reduction of the imido group in the Schiff's base compounds. The procedure was applied to the determination of lysine and arginine in foodstuffs and the total proteins in serum samples.     

Determination of alcohol dehydrogenase activity by differential pulse polarography (DPP)

Conclusion With the aid of the differential pulse polarographic assay, the alcohol dehydrogenase activity can be measured in rat liver tissue and human serum with a high degree of sensitivity and accuracy (ranging from 1 to 200 U/l).

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Bestimmung der Alkohol-Dehydrogenase mit Hilfe der Differential-Pulse-Polarographie (DPP)

     

Differential-pulse polarographic determination of N-nitrosoproline in uncooked meat

Ham and bacon have been analysed for N-nitrosoproline by differential-pulse polarography. Quantitative polarograms without interfering peaks were obtained from ethanol extracts prepared after extensive clean-up which included freeze-drying and column chromatography. Differential-pulse polarography proved sufficiently sensitive to give peaks corresponding to ca. 100 mug of N-nitrosoproline per kg in several commercial samples of cured meat.     

Differential-pulse polarography of trichothecene mycotoxins : Determination of Deoxynivalenol,Nivalenol and Fusarenone-X in Maize

The polarographic behaviour of representative trichothecenes is described. Compounds characterized by an α,β-unsaturated carbonyl group or by a macrocyclic lactonic ring were found to be electroactive in a methanolic Britton—Robinson buffer. Differential pulse polarography provides detection limits of the order of 40 nmol l^?1 with linear ranges extending up to 9 μmol l^?1. The application of differential pulse polarography is described for the determination of nivalenol (3α, 4β, 7α, 15-tetrahydroxy-12,13-epoxytrichotec-9-en-8-one), deoxynivalenol (3α, 7α, 15-trihydroxy-12,13-epoxytrichothec-9-en-8-one) and fusarenone-X (3α, 7α, 15-trihydroxy-4 β-acetoxy-12,13-epoxytrichothec-9-en-8-one) in infected maize. A suitable liquid/liquid extraction and chromatographic cleanup procedure is reported. Detection limits for the overall procedure and for a sample size of 50 g are of the order of 50 ng g^?1 while average recoveries range from 20 to 70% at the 1 μg g^?1 level. Polarographic results are compared with those obtained by a gas-chromatographic method.     

HPTLC method for determination of nevirapine in pharmaceutical dosage form

A sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic method of analysis of nevirapine both as a bulk drug and in formulations was developed and validated. The solvent system consisted of toluene-carbon tetrachloride-methanol-acetone-ammonia (3.5:3.5:2.0:1.0:0.05, v/v/v/v/v). Densitometric analysis of nevirapine was carried out in the absorbance mode at 289nm. This system was found to give compact spots for nevirapine (R(f) value of 0.44+/-0.02). Nevirapine was subjected to acid and alkali hydrolysis, oxidation, dry heat and wet heat treatment and photodegradation. The drug undergoes degradation under acidic, basic conditions and oxidation. Also the degraded products were well resolved from the pure drug with significantly different R(f) values. Linearity was found to be in the range of 30-1000ng/spot with significantly high value of correlation coefficient. The linear regression analysis data for the calibration plots showed good linear relationship with r(2)=0.998+/-0.002 in the working concentration range of 300ng/spot to 1000ng/spot. The mean value of slope and intercept were 0.073+/-0.005 and 36.78+/-1.50, respectively. The method was validated for precision, robustness and recovery. The limit of detection and quantitation were 5 and 10ng/spot, respectively. As the method could effectively separate the drug from its degradation products, it can be employed as a stability indicating one. Moreover, the proposed HPTLC method was utilized to investigate the kinetics of acid degradation process. Arrhenius plot was constructed and activation energy was calculated.     

Differential-pulse polarographic determination of selenium species in contaminated waters

Selenium(IV), in the concentration range 2–100 μg l^?1 in contaminated waters, is determined by using the sensitive adsorption-controlled peak obtained by differential pulse polarography in dilute acid solution. Interfering heavy metals are removed on Chelex-100 resin. Selenium(VI) is not electroactive but can be determined after photolytic reduction in the absence of oxygen. Anion-exchange preconcentration is necessary if the total selenium is below the detection limit of 2 μg l^?1.     

Monitoring of Zn(II) and Cd(II) adsorption on activated carbon from aqueous multicomponent solutions by differential pulse polarography (DPP)

The adsorption process of Zn(II) and Cd(II) from aqueous solution has been investigated from both kinetic and equilibrium standpoints, using differential pulse polarography (DPP) on a mercury dropping electrode as the analytical technique. With such an aim, adsorption experiments were performed using not only a single metal ion–Zn(II) or Cd(II) solution but also a multi-component ion metal–Zn(II), Cd(II) and Hg(II) solution. The influence of the pH change in the multi-component ion metal solution on the adsorption of Zn(II) and Cd(II) was also studied. The adsorption processes is relatively fast for Zn(II) and Cd(II). The presence of two foreign ions in the solution slightly speeds up the adsorption process for Zn(II) and significantly slows it down for Cd(II). The adsorption isotherms are similarly shaped for Zn(II) and Cd(II). The addition of the foreign ions has a more unfavourable effect on the adsorption for Cd(II) than for Zn(II). At pH 2, neither Zn(II) nor Cd(II) is adsorbed practically on the carbon. The voltammetric approach has proved to be a fast and efficient method that, at the same time, enables one to monitor the adsorption of Zn(II) and Cd(II) with potential on-line application, which could be useful in waste-water treatment.     

Differential-pulse polarographic determination of the insecticide imidacloprid in commercial formulations

The reduction reaction of imidacloprid [1-(6-chloro-3-pyridylmethyl)-N-nitroimidazolidin-2-ylideneamine] at a mercury electrode shows two well-defined waves in the range of pH 2.0–11.0. The characteristics of the electrode processes were examined. The analyte captures four electrons in the first step and two in the second to give the hydroxylamine and amine derivatives, respectively. A differential-pulse polarographic method for the determination of imidacloprid based on the first reduction peak of this compound is presented. Britton-Robinson buffer was used as a supporting electrolyte and optimum pH value was found to be pH 8.O. The applicable concentration range was from 10 to 200 ng/ml, with a relative standard deviation of 1.5% (for a level of 80 ng/ml) and a detection limit of 3 ng/ml. The method has been satisfactorily applied to the determination of imidacloprid in commercial formulations.     

Differential-pulse polarographic determination of chromium and nickel in zircaloys using microsamples

Three methods were developed for the analysis of the alloying elements chromium and nickel in Zircaloy-2 and Zircaloy-4, alloys of zirconium used extensively in the nuclear industry as nuclear fuel sheathing. Zircaloy was dissolved in hydrofluoric acid followed by oxidation of Cr(III) to Cr(VI) by perchloric acid. The polarographic peak of CrO ₄ ^2– in alkaline medium was used to determine Cr. Nickel was determined, after HF dissolution, using the polarographic peak of the nickel-ammonia complex, Ni (NH₃) ₆ ²⁺ . In an alternative method for Ni, the sample was dissolved in HF and the polarographic peak of the nickel-fluoride complex, NiF ₄ ^2– , was used. Careful control of fluoride ion concentration and the pH eliminated the harmful effect of fluoride on the capillary behaviour of the dropping mercury electrode. The detection limits for chromium, nickel-ammonia and nickel-fluoride in Zircaloys were 0.0016, 0.0033, and 0.0041%, respectively.     

The determination of chromium(VI) in natural waters by differential pulse polarography.

A method utilizing differential pulse polarography for the determination of chromium(VI) in natural water is described. Additions of 0.62 μg Cu(II) ml^-1 and 0.55 μg Fe(III) ml^-1 did not interfere with the determination of 0.050 μg Cr(VI) ml^-1. The natural water samples containing chromium(VI) were buffered to approximately pH 7 with 0.1 M ammonium acetate and 0.005 M ethylene diamine and analyzed. Natural water samples of chromium content from 0.035 μg ml^-1 to 2.0 μg ml^-1 may be analyzed directly without further preparation. The detection limit is 0.010 μg ml^-1.     

Some electroanalytical aspects of using pulse polarography for determination of Ge(IV)

Summary Presented data give some informations of analytical importance as a result of pulse polarographic investigations of Ge(IV) in KCl solutions within pH range 3–12 at Ge concentration from 1×10^–4 to 2.5×10^–6 M. It was shown that Ge(IV) can be polarographically active in acidic solution but its reduction interferes with hydrogen gas development. The addition ofp-quinone enables the determination of Ge(IV) without this interfering effect.Suggested explanation of the observed changes in polarographic curves dependent on pH and Ge concentration based on the existence of several polarographically active forms.

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Elektroanalytische Bemerkungen zur pulspolarographischen Bestimmung von Ge(IV)

Zusammenfassung Unsere Ergebnisse bieten einige Informationen über die pulspolarographische Bestimmung von Ge(IV) in KCl-Lösungen innerhalb pH 3–12 und bei Ge-Konzentrationen zwischen 10^–4 und 2,5×10^–6 M. Es wurde gezeigt, daß Ge(IV) in saurer Lösung polarographisch aktiv ist, seine Reduktion aber durch Wasserstoff-Entwicklung gestört wird. Der Zusatz vonp-Chinon beseitigt diese Störung. Die Änderung der polarographischen Kurven je nach Ge-Konzentration und pH beruht vermutlich auf der Existenz verschiedener polarographisch aktiver Formen.

     

Spectrophotometric simultaneous determination of rabeprazole sodium and itopride hydrochloride in capsule dosage form

A new simple, economical, rapid, precise and accurate method for simultaneous determination of rabeprazole sodium and itopride hydrochloride in capsule dosage form has been developed. The method is based on ratio spectra derivative spectrophotometry. The amplitudes in the first derivative of the corresponding ratio spectra at 231nm (minima) and 260nm were selected to determine rabeprazole sodium and itopride hydrochloride, respectively. The method was validated with respect to linearity, precision and accuracy.