


Vol 79, No 12 (2024)
REVIEWS
Application of the X-ray fluorescence method in Russia to study the chemical composition of medical plants
Abstract
The use of X-ray spectral analysis in determining the elemental composition of medicinal plants have been considered. The review mainly presents works by Russian authors published in Russian journals and collections over the past 20 years. When determining the contents of macro- and microelements in medical plants, the authors utilize X-ray fluorescence spectrometry (XRF) with wavelength dispersion (WDXRF), with energy dispersion (EDXRF), synchrotron radiation XRF (SR XRF), total reflection XRF (TXRF), electron probe microanalysis and scanning electron microscopy. The simultaneous determination of macro- and microelements, a non-destructive sample preparation procedure and acceptable time and reagent expenses make XRF attractive in the identification and control of the chemical composition of plants, in particular, those used in medical practice. Most of the published works contain information on the sample preparation and measurement procedures, metrological estimates are given and the results obtained are discussed. However, there is no methodological information in some publications. There are typos in the presentation of analytical data.



ORIGINAL ARTICLES
Sorption concentration of flavonoids by ordered mesoporous silica synthesized in the presence of a potential sorbate
Abstract
The use of nanostructured sorbents at the stages of sample preparation (extraction, concentration) of multicomponent mixtures in the processes of solid-phase extraction of organic substances is of great interest. In the present work, the sorption properties of ordered mesoporous analogues of SBA-15 synthesized in the presence of quercetin as a potential sorbate are studied. The features of sorption isolation and concentration of quercetin, dihydroquercetin, naringin and rutin under dynamic conditions from acetonitrile solutions by the method of breakthrough curves are considered. The use of a generalized criterion for optimizing the sorption concentration of CE within the framework of the model of dynamic sorption concentration of Venitsianov – Tsyzin, taking into account the limiting (mixed-diffusion) stage of sorption kinetics, made it possible to evaluate the effectiveness of sorption concentration of flavonoids on the studied sorbents. It is shown that the use of ordered silica synthesized in the presence of a potential sorbate makes it possible to significantly increase the concentration efficiency compared with unstructured silicas, as well as samples of an unmodified analogue of SBA-15.



Pyridine-2,6-dicarboxylic acid esters – new ligands for extraction and determination of metals
Abstract
N,O-Hybrid donor ligands are promising compounds for the isolation and separation of actinides and lanthanides from technological solutions during the processing of spent nuclear fuel. New synthesized N,O-hybrid donor ligands – derivatives of 2,6-pyridindicarboxylic acid – have been studied as extractants and membrane components for potentiometric sensors. The extraction ability of solutions of these compounds in meta-nitrobenzotrifluoride with respect to d- and f-elements from solutions of nitric and perchloric acids has been studied. It has been shown that the replacement of a mide groups with ester groups reduces the extraction ability of ligands. The transition from nitric acid to chloric acid gives a sharp increase in the extraction capacity due to the perchlorate effect. A significant increase in the extraction capacity is also observed when chlorinated cobalt dicarbollide is added to the organic phase: the highest distribution coefficient is obtained with a ratio of the concentrations of the extractant and the additive 1:1. Potentiometric membrane sensors based on new ligands have demonstrated significant sensitivity to Cd2+. The correlation between the behavior of new ligands in extraction and in potentiometric measurements has been studied.



Determination of urea and humate in humate fertilizers by IR-FTIR spectroscopy
Abstract
Conditions for determining the content of urea and humates in aqueous fertilizers in their combined pr esence by IR spectroscopy of frustrated total internal reflection are proposed. The urea and humate spectra were identified. Characte ristic bands of urea and humate were selected for their determination in the joint presence. The error in determining urea is minimal w hen registering an analytical signal at 1628 and 1598 cm–1 (10-200 g/l), humate — at 1380 cm–1 (10-100 g/l). When calculating the content of humate and urea in their mixtures by the Firordt method, the e rror in determining each component is 3%. The proposed determination conditions have been tested on model fertilizers and commercial humate fertilizers.



Non-destructive testing of macrolides in tablet medicines by near-infrared fourier spectroscopy and digital colorimetry
Abstract
Non-destructive testing of the active substances azithromycin and clarithromycin in tablet medicines without opening the blister pack by measuring the intensity of diffuse reflection of IR radiation is proposed. Two methods were used – near-infrared spectroscopy with Fourier transform and colorimetry using a smartphone and a 3D-printed device. The data array (IR diffuse reflection spectra, digital values of colorometric channels) was processed using principal component methods, hierarchical cluster analysis and partial least squares regression using TQ Analyst, PhotoMetrix PRO® software. The use of chemometric algorithms to determine the concentration of the active substance and identify the manufacturer of medicinal products is considered. IR spectroscopy and colorimetry methods have shown equivalent results in identifying the manufacturer of medicines and determining the concentration of active substances in tablets without opening the blister pack.



Determination of polystyrene nanoparticles in aqueous solutions by the method of two-beam thermolens spectrometry
Abstract
Polymer micro- and nanoparticles (microplastics) are an environmental pollutant. The low content of microplastics in such objects can affect ecosystems and human health, therefore, there is a growing need to determine microplastic particles at a low content level and simultaneously assess the physico-chemical parameters of the systems under study. Thermolensing spectrometry (TLS) was used to determine polystyrene particles with sizes of 65 and 80 nm in the concentration range of 0.0005–0.15 mg/l in their aqueous dispersions. The comprehensive registration of the TL data also made it possible to evaluate the thermal conductivity of these solutions. It has been established that an increase in the content of polystyrene nanoparticles in water leads to a nonlinear change in thermal conductivity.



Microextraction-chromatographic determination of furan derivatives in transformer oil
Abstract
An express and environmentally safe method has been developed for microextraction of furan derivatives from transformer oil for their determination by high-performance liquid chromatography with spectrophotometric detection in the ultraviolet region of the spectrum. Various hydrophilic eutectic solvents have been studied as extractants for the implementation of dispersion liquid-liquid microextraction with vortex dispersion. It was found that the highest values of the degree of extraction (from 85 to 96 %) are provided by a three-component eutectic solvent based on choline chloride, acetic acid and water. The rapid spontaneous phase separation made it possible to eliminate the centrifugation stage. Detection limits (3σ) from 1 to 5 micrograms/l have been reached.



Batch-injection amperometric determination of sulfamethazine, sulfacetamide and sulfathiazole on an electrode modified with a composite based on gold particles, carbon nanotubes and ionic liquid
Abstract
Electrodes modified with gold particles, multi-walled carbon nanotubes, an ionic liquid based on 1-butyl-3-methylimidazolium hexafluorophosphate, as well as a composite based on them for the voltammetric determination of sulfamethazine, sulfacetamide and sulfathiazole have been developed. It has been established by cyclic voltammetry that modification of the surface of a glass-carbon electrode with gold particles, a composite based on carbon nanotubes and an ionic liquid leads to an increase in its effective area. The electrochemical impedance data indicate an increase in the electron transfer rate on the modified electrodes compared to the unmodified one. A composite electrode with gold particles, carbon nanotubes and an ionic liquid with the best characteristics was used for the amperometric determination of sulfonamides under batch injection conditions. The optimal parameters for the determination of sulfonamides in the batch injection system have been established. The dependence of the analytical signal on the concentration of the compounds in question in logarithmic coordinates is linear in the range from 1 × 10–8 to 5 × 10– 3 M for sulfamethazine and sulfacetamide and from 1 × 10–7 to 5 × 10–3 M for sulfathiazole. The proposed method for the determination of sulfonamides has been tested in the analysis of medicines.



Voltammetric DNA sensors for detecting DNA damage based on poly (acridine orange) coatings obtained from relin and glycelin
Abstract
A voltammetric DNA sensor has been developed to register DNA damage from the calf thymus by changing redox signals on cyclic voltammograms of a poly (acridine orange) (PAO) coating synthesized on a printed carbon-containing electrode from media of deep eutectic solvents – relin and glycelin and a phosphate buffer solution. The working conditions of DNA immobilization on each of the presented polymer coatings have been established. The influence of the nature of the electropolymerization medium on the electrochemical characteristics of the polymer acridine dye layer and the sensitivity of the polymer response to thermal and oxidative DNA damage has been revealed. With the optimal composition of the surface layer, the DNA sensor based on PAO synthesized from aqueous media (PAO1) reliably allowed us to determine only the fact of chemical oxidation of DNA. The use of PAO synthesized from relin (PAO2) and glycelin (PAO3) media in DNA sensors demonstrated not only the high sensitivity of PAO2 and PAO3 coatings to the introduction of DNA from the thymus of the calf as a whole, but also made it possible to successfully distinguish native, thermally denatured and chemically oxidized DNA.



IN THE SCIENTIFIC COUNCIL FOR ANALYTICAL CHEMISTRY OF THE RAS
48th Annual Council Session



Opening speech by Academician Y.A. Zolotov, Chairman of the Scientific Council of the Russian Academy of Sciences for Analytical Chemistry at the Annual Session of the Council on June 27, 2024



About Russian Departments of Analytical Chemistry



EVENTS
Anniversary of Professor E.G. Kulapina


