Dragan S. Veselinović

Antioxidant activity of propolis extracts from Serbia: A polarographic approach

Antioxidant activity (AO) of commercial propolis extracts (PEs), available on Serbian market, was determined by direct current (DC) polarography. Polarographic anodic current of 5.0 mmol L(-1) alkaline solution of H2O2 was recorded at potentials of mercury dissolution. Decrease of the current was plotted against the volume of gradually added PEs. The volume of PE causing 20% current decrease was determined from the linear part of the plot. Antioxidant activity was expressed in H2O2 equivalent (HPEq), representing the volume of PE that corresponds to 1.0 mmol L(-1) H2O2 decrease. Resulting HPEq ranged between 1.71±0.11 and 8.00±0.18 μL. Range of 1,1-diphenyl-2-picryl hydrazyl (DPPH) radical scavenging activity was from 0.093±0.004% to 0.346±0.006%. Total phenolic content (TCP) of PE with superior AO activity was 5.31±0.05% g GAE, while the extract with the lowest activity contained 1.45±0.02% g GAE. Antioxidant activity, determined by polarographic method, was correlated with DPPH scavenging activity (R2=0.991) and TCP (R2=0.985). Validity of obtained results was further confirmed using ANOVA and post hoc Tukey HSD test.

Spectrophotometric determination of pefloxacin in pharmaceutical preparations

It has been established that the antibiotic pefloxacin (Abaktal) methanesulphonate reacts with Fe(III) at pH 1.00-8.00 to form a water-soluble complex with maximum absorbance at 360 nm. The composition of the complex, determined spectrophotometrically by the application of Jobs, molar-ratio and Bent-Frenchs methods, was pefloxacin: Fe(III) = 1:1 (pH = 2.50; lambda = 360 nm; mu = 0.1 M). The relative stability constant, obtained by the methods of Sommer and Asmus was 10(5.02) (pH = 2.50; lambda = 360 nm; mu = 0.1 M). The molar absorptivity of the complex at 360 nm was found to be 4.8 x 10(3) l mol-1 cm-1. Beers law was followed for pefloxacin concentrations of 2.15-85.88 micrograms ml-1. The lower sensitivity limit of the method was 2.15 micrograms ml-1. The relative standard deviation (n = 10) was 0.57-1.07%. The method can be applied to the rapid and simple determination of pefloxacin in aqueous solutions and tablets.

Spectrophotometric determination of oxytetracycline in pharmaceutical preparations using sodium molybdate as analytical reagent

Abstract A spectrophotometric method is proposed for the determination of oxytetracycline in pharmaceutical preparations. The method is based on the measurement of the absorbance of the molybdate—oxytetracycline complex at 404 nm (pH 5.50; μ = 0.1 M; 20°C). The composition of the complex (1:1) was determined by the application of the spectrophotometric methods of Job and Bent—French (pH 5.50; λ = 390 nm; μ = 0.1 M). The relative stability constant ( K ′ = 10 4.6 ) of the complex was obtained by the methods of Sommer and Nash (pH 5.50; λ = 390 nm; μ = 0.1 M; 20°C). The molar absorptivity of the complex was 9.5 × 10 3 l mol −1 cm −1 . Beers law was obeyed over the concentration range 2.48–34.78 μg ml −1 . The relative standard deviation RSD ( n = 10) was 0.27–0.39%. The method proposed can be applied to the assay of oxytetracycline in capsules. The detection limit of oxytetracycline is 2.5 μg ml −1 .

Potentiometric and spectrophotometric determination of the dissociation constants of cefetamet

SummaryThe dissociation constants of cefetamet-Na have been determined using potentiometric titrations and spectrophotometry. The investigations were carried on in water solutions at constant temperature and ionic strength, and at differentH0 andpH values. Potentiometric investigations were performed at three different temperatures and ionic strengths. The concentration dissociation constants and the corresponding thermodynamic dissociation constants were calculated by a computer program. The mixed dissociation constants (pK′) of cefetamet-Na have been determined spectrophotometrically in theH0 range from -5.80 to 0.00 and atpH values from 0.00 to 12.70 and are in good agreement with values achieved by graphical methods as well as with those obtained by potentiometric methods. Based on the determined values, the thermodynamic parameters (ΔG, ΔH, ΔS) were calculated atI=0.1M.ZusammenfassungDie Dissoziationskonstanten von Cefetamet-Na wurden mittels potentiometrischer Titrationen und auf spektrophotometrischem Weg bestimmt. Die Untersuchungen wurden in wäßriger Lösung bei konstanter Temperatur und Ionenstärke und verschiedenenH0- undpH-Werten durchgeführt. Potentiometrische Messungen wurden bei drei verschiedenen Temperaturen und Ionenstärken vorgenommen. Die stöchiometrische Dissozation und die entsprechenden thermodynamischen Dissoziationskonstanten wurden mit Hilfe eines Computerprogramms berechnet. Die gemischten Dissoziationskonstanten (pK′) wurden spektrophotometrisch imH0-Bereich von -5.80 bis 0.00 und impH-Bereich von 0.00 bis 12.70 bestimmt und stimmen sowohl mit Werten, die mit Hilfe der graphischen Methode erhalten wurden, als auch mit potentiometrisch bestimmten gut überein. Aus den ermittelten Werten der Dissoziationskonstanten wurden die thermodynamischen Parameter (ΔG, ΔH, ΔS) fürI=0.1M berechnet.

Polarographic investigation of the Cu(II) complex with ampicillin

The complex of Cu(II) ion and ampicillin is investigated polarographically in aqueous medium, at pH = 6, an ionic strength μ = 0.2, and room temperature. The stoichiometric ratio of Cu(II) and ampicillin in the complex, and the stability constant, logK′ = 5.1, were determined by Linganes method.

Differential Pulse Polarographic Investigation of Copper (II) - Cephalexin Complex

Abstract It has been found by dp polarography that cephalexin forms a complex Cu(CEF)2, at pH = 8.7, ionic strength μ = 0.2 and room temperature. The stoichiometric ratio and stability constant values have been evaluated by Linganes and De Ford and Humes methods. The overall stability constants, logβ2 = 9.44 and 9.13, have been determined with methods applied.

Desorption of 137Cs from Brachythecium mildeanum moss using acid solutions with pH 4.60–6.50

The desorption of 137Cs from the moss Brachythecium mildeanum (Schimp.) was performed using the following solutions: H2SO4 (I), HNO3 (II), H2SO4 + HNO3 (III) with pH values of 4.60, 5.15, and 5.75, respectively, as well as distilled water (D) with pH 6.50. After five successive desorptions, each lasting 24 h, 20.5–37.6% 137Cs was desorbed from the moss using these solutions, while 30.7% of the starting content was desorbed using distilled water. The first desorption removed the highest percent of the original content of 137Cs in the moss (11.3–18.4%). This was determined by measuring 137Cs activity. If the current results are compared with those obtained earlier it may be concluded that 137Cs desorption from mosses is not species-dependent. The obtained results indicate the necessity of investigating the influence of acid rain, or rather, of H+ ions, on desorption of other ions from biological systems, i.e., the role of H+ ions in spreading other polluting compounds and thus producing secondary environmental pollution. From the results of this study it follows that acid rain will lead, through H+ ion action, to a similar increasing pollution of fallout waters with other ionic compounds which may not be present in the water before the contact with the plants and thus enable the pollution spreading. In the investigated system, the replacement of H+ ions from acid rains by more dangerous radioactive ions occured, increasing the concentration of the radioactive ions in the water, which demonstrates that the same process takes place in fallout water.

137Cs desorption from lichen using acid solutions

Desoprtion of 137Cs from samples of Cetraria islandica lichen using HCl (A) and HNO3 (B) acid solutions with pH values from 2.00 to 3.75 was investigated. After five consecutive desorptions lasting 24 h it was shown that between 52.2% (solution B pH 3.28) and 72.2% (solution A pH 2.00) of 137Cs was desorbed from the lichen and the initial desorptions were the most successful. Lichen desorbed with the stated solutions did not undergo structural changes. The amount of absorbed water from solutions A and B, used for desorption from lichen, in relation to the starting volume (expressed in %) showed that solution concentration did not take place. Lichen act as neutralizing agents because the pH of the lichen thallus is higher than the pH value of the solution used

Spectroscopic and Theoretical Study of Cyanidin–Aluminum (III) Complexes

Abstract Complexation of aluminum (III) with cyanidin, a natural anthocyanidin molecule, has been investigated in methanol and buffered solutions of pH 3.0 and 4.0. Electronic absorption spectroscopy was performed to characterize the stoichiometry and stability of the complexes formed. In investigated solvents, aluminum bonded moderately to cyanidin requiring large mole ratios of the components (up to 200) for the access of complexation. Molar ratio plots showed the formation of only one complex with stoichiometry aluminum (III):cyanidin of 1∶1 in both investigated media. Semiempirical calculations, performed in the Austin Model 1 parameterization, enabled the determination of the structural features of free compounds as well as complex structural modifications caused by chelation of Al(III).

Chiral ligand-exchange chromatography as the screening method for proposed modifications in exametazime synthesis to enhance diastereoselectivity

99M Tc (V)-d,l-HM-PAO complex is well-known radiopharmaceutical for regional cerebral blood flow imaging. The proposed modifications in exametazime, hexamethylpropyleneamine oxime (HM-PAO) (4,8-diaza-3,6,6,9-tetramethylundecane-2,10-dione bisoxime) synthesis, for reduction of intermediary reactant diiminebisoxime (DI) (4,8-diaza-3,6,6,9-tetramethylundecane-3,8-diene-2,10-dione bisoxime) concerned two reductants (NaBH(4) and KBH(4)), two solvents (ethanol and 2-propanol), and three mole ratios of reactant/reductants (1:1, 1:1.5, and 1:2). The simultaneous analysis of diastereo-enantiomeric HM-PAO content, as well as the content of starting DI, in different reduction mixtures were performed using chiral ligand-exchange chromatography (CLEC). The separation of the samples of investigated reduction mixtures, obtained in the second step of HM-PAO synthesis, has been accomplished by using an achiral sorbent (RP-18) and a chiral mobile phase (CMP) containing copper(II) complex with N,N-dimethyl-l-phenylalanine (l-DM-PhA) as initial complex for CLEC. With 12 different reduction conditions, the obtained ratios of diastereoisomers d,l-HM-PAO: meso-HM-PAO varied from 69.2:30.8 to 15.9:84.1, in comparison to the reduction in routine synthesis of HM-PAO which gives an equal mixture of diastereoisomers. The ternary mixed complexes formation recorded spectrophotometrically on addition of HM-PAO or DI to the mobile phase with binary complex Cu(l-DM-PhA)(2), due to the evidence of bathochromic shift of 46nm for lambda(max) with significant difference in absorptivity contributes to separation mechanism.