Study of the Retention Behavior of Newly Synthesized s-Triazine Derivatives in RP TLC Systems,and the Lipophilicity of the Compounds

JPC – Journal of Planar Chromatography – Modern TLC - The chromatographic behavior of nine newly synthesized s-tri-azines has been studied by thin-layer chromatography on C18/UV254...     

Real-time polymerase chain reaction detection of cauliflower mosaic virus to complement the 35S screening assay for genetically modified organisms

Labeling of genetically modified organisms (GMOs) is now in place in many countries, including the European Union, in order to guarantee the consumer's choice between GM and non-GM products. Screening of samples is performed by polymerase chain reaction (PCR) amplification of regulatory sequences frequently introduced into genetically modified plants. Primers for the 35S promoter from Cauliflower mosaic virus (CaMV) are those most frequently used. In virus-infected plants or in samples contaminated with plant material carrying the virus, false-positive results can consequently occur. A system for real-time PCR using a TaqMan minor groove binder probe was designed that allows recognition of virus coat protein in the sample, thus allowing differentiation between transgenic and virus-infected samples. We measured the efficiency of PCR amplification, limits of detection and quantification, range of linearity, and repeatability of the assay in order to assess the applicability of the assay for routine analysis. The specificity of the detection system was tested on various virus isolates and plant species. All 8 CaMV isolates were successfully amplified using the designed system. No cross-reactivity was detected with DNA from 3 isolates of the closely related Carnation etched ring virus. Primers do not amplify plant DNA from available genetically modified maize and soybean lines or from different species of Brassicaceae or Solanaceae that are natural hosts for CaMV. We evaluated the assay for different food matrixes by spiking CaMV DNA into DNA from food samples and have successfully amplified CaMV from all samples. The assay was tested on rapeseed samples from routine GMO testing that were positive in the 35S screening assay, and the presence of the virus was confirmed.     

Evaluation of RP-HPLC Method Intended for the Analysis of Cefuroxime Axetil and ITS Impurities Supported by Experimental Design

In this paper, a chemometrically assisted validation of RP-HPLC method, intended for the quantitative analysis of cefuroxime axetil (A and B), cefuroxime acid, cefuroxime lactone, cefuroxime axetil sulfoxide (A and B), ?³-cefuroxime axetil and anti cefuroxime axetil (A and B) in tablets, is presented. Since the successful separation could be achieved with the mobile phase containing only methanol and water, Luna C18 column was selected for the analysis. Under these circumstances, the optimization was quite straightforward and included only a fine tuning of the chromatographic conditions to reduce total run time and maintain the achieved separation. The established method was then subjected to the method validation and the required validation parameters were tested. For the robustness evaluation, a fractional factorial 2^4?1 design was utilized and factors that might significantly affect the system performance were defined. For the significant factors, the non-significant intervals were determined and the acceptable system suitability limit for resolution factor between cefuroxime axetil A and cefuroxime axetil ?³ isomer (R ₂) was calculated. As the other validation parameters were also found to be suitable, the possibility to apply the proposed method for the determination of cefuroxime axetil, cefuroxime acid, cefuroxime lactone, cefuroxime axetil sulfoxide, ?³-cefuroxime axetil and anti cefuroxime axetil in any laboratory under different circumstances is proven.     

Radionuclide concentrations in samples of medicinal herbs and effective dose from ingestion of ¹³⁷Cs and natural radionuclides in herbal tea products from Serbian market

The objective of this study is to evaluate natural and artificial radioactivity levels in 18 different samples of medicinal herbs from Serbian market. The activity concentrations of (238)U, (232)Th, (40)K, and (137)Cs were measured using gamma spectroscopy system with a high-purity germanium detector. The activity concentrations of (238)U, (232)Th, (40)K, and (137)Cs were found to be in a range of 0.6-8.2, 1.7-15.1, 126-1243.7, and 0.3-8.8 Bq/kg, respectively. The annual whole body doses from ingestion of (137)Cs and natural radionuclides for an adult person who consumed herbal tea from these medicinal herbs were found to be 2.5-469.9 nSv for (137)Cs, 0.7-9.7 nSv for (238)U, 0.3-2.8 nSv for (232)Th, and 1026.0-10,132.0 nSv for (40)K. These doses are not hazardous to public health. The obtained results were compared with correspondent studies conducted worldwide.     

Simultaneous Determination of Pb and Cd Traces in Water Samples by Anodic Stripping Voltammetry Using a Modified GC Electrode

The determination of Pb and Cd with a Nafion‐modified glassy carbon electrode and Cu‐DPABA complex (Cu‐DPABA–NA/GCE; DPABA is methyl 3,5‐bis{bis‐[(pyridin‐2‐yl)methyl]amino}methyl‐benzoate) as an alternative electrode for anodic stripping voltammetry was described. Pb and Cd were accumulated in acetate buffer pH 4 at a potential of ?1.4 V (vs. Ag/AgCl electrode) for 120 s followed by a DPASV scan from ?1.2 to ?0.2 V. Under optimum conditions the calibration curves were linear in the range of 4.8×10^?9–5.0×10^?5 and 5.0×10^?9–5×10^?5 mol L^?1 for Pb and Cd, respectively. Detection limits were 1.8×10^?9 and 1.2×10^?9 mol L^?1 for Pb and Cd, respectively. Different parameters and conditions, such as membrane ingredients, accumulation time, potential and pH value were optimized. A study of interfering substances was also performed. A significant increase in current was achieved at the modified electrode in comparison with the bare glassy carbon electrode. The validation of the proposed method was made by Pb and Cd determination in the certified reference material Groundwater CRM 610 (BCR, Community Bureau of Reference, Brussels, Belgium). The electrode was successfully applied for determination of Pb and Cd in river water with a high content of organic contaminants without any pretreatment.     

Removal of nickel(II) ions from aqueous solutions using the natural clinoptilolite and preparation of nano-NiO on the exhausted clinoptilolite

The natural zeolite tuff (clinoptilolite) from a Serbian deposit has been studied as adsorbent for Ni(II) ions from aqueous solutions. Its sorption capacity at 298 K varies from 1.9 mg Ni g⁻¹ (for the initial solution concentration of 100 mg Ni dm⁻³) to 3.8 mg Ni g⁻¹ (for C₀ = 600 mg Ni dm⁻³) and it increases 3 times at 338 K. The sorption is best described by the Sips isotherm model. The sorption kinetics follows the pseudo-second-order model, the activation energies being 7.44, 5.86, 6.62 and 6.63 kJ mol⁻¹ for C₀ = 100, 200, 300 and 400 mg Ni dm⁻³, respectively. The sorption involves a film diffusion, an intra-particle diffusion, and a chemical cation-exchange between the Na⁺ ions of clinoptilolite and the Ni²⁺ ions. The sorption is endothermic (ΔH° being 37.9, 33.4, 30.0, 27.7 and 24.3 kJ mol⁻¹ for C₀ = 100, 200, 300, 400 and 600 mg Ni dm⁻³, respectively) and spontaneous in the 298-338 K temperature range. Thermal treatment of the Ni(II)-loaded clinoptilolite results in the formation of spherical nano-NiO particles of approx. 5 nm in diameter which are randomly dispersed in the clinoptilolite lattice.     

Analysis of Velázquez’s solution to the mean curvature flow with a type II singularity

Velázquez in 1994 used the degree theory to show that there is a perturbation of Simons’ cone, starting from which the mean curvature flow develops a type II singularity at the origin. He also showed that under a proper time-dependent rescaling of the solution around the origin, the rescaled flow converges in the C⁰ sense to a minimal hypersurface which is tangent to Simons’ cone at infinity. In this paper, we prove that the rescaled flow actually converges locally smoothly to the minimal hypersurface, which appears to be the singularity model of the type II singularity. In addition, we show that the mean curvature of the solution blows up near the origin at a rate which is smaller than that of the second fundamental form.