Ашық рұқсат Ашық рұқсат  Рұқсат жабық Рұқсат берілді  Рұқсат жабық Тек жазылушылар үшін

Том 80, № 3 (2025)

Мұқаба

Бүкіл шығарылым

Ашық рұқсат Ашық рұқсат
Рұқсат жабық Рұқсат берілді
Рұқсат жабық Тек жазылушылар үшін

REVIEWS

Chemical analysis on the way to a consumer: solutions for food quality control

Apyari V., Zolotov Y., Dmitrienko S., Furletov A., Tikhomirova T.

Аннотация

One of the pronounced trends in modern analytical chemistry is increasing availability of chemical analysis for mass consumers. By now, a large number of produced test kits for semi-quantitative analysis and a number of devices for evaluation of compliance of individual parameters of the analyzed object with the required standards have appeared. The review systematizes and discusses the main existing solutions in this field today, proposed for food analysis, and reflects the current state of the art in this area. According to the authors opinion, the concept of accessibility of this or that accessory is largely determined by its availability on the market and its acceptable cost for an individual buyer, so the review focuses on commercialized analytical tools costing mainly up to 100 thousand rubles. Relatively inexpensive and easy-to-use test tools, portable electrochemical, spectroscopic, refractometric, ultrasonic systems, as well as electronic nose type systems for chemical analysis are considered, their main characteristics and approximate cost are given. Suggestions are made about the prospects of further development of chemical analysis instruments available for mass consumers.

Zhurnal Analiticheskoi Khimii. 2025;80(3):235-253
pages 235-253 views

ORIGINAL ARTICLES

Separation of microplastics from river water in a rotating spiral column using a water-oil system

Ermolin M., Ivaneev A., Savonina E., Dzhenloda R.

Аннотация

Determination of microplastic content in natural waters is an urgent task in assessing the degree of pollution of water bodies, identifying sources of pollution, as well as in assessing potential risks for inhabitants of aquatic ecosystems and water consumers. The solution of such a problem mainly lies in the field of analytical chemistry, with particle separation methods playing the most important role. The present work shows for the first time the possibility of applying the method of flowing microplastic separation in a rotating spiral column using a water-oil system to assess the content of microplastics in river water. Microplastics in the extracted particle samples were determined by pyrolysis gas chromatography with mass spectrometric detection (Pyro-GC-MS). A water sample from the Moskva River was analyzed. Using the water-castor oil system, 1.8 mg/L of suspended solids were separated from river water. The decomposition procedure of the organic matter (30 % H2O2) of the sample reduced the mass of extracted particles to 0.4 mg/L. The residual fraction was studied by optical microscopy. According to the Pyro-GC-MS data, the total content of microplastics in the studied water sample was 109 µg/L, which is 1.4 % of the total suspended solids in the studied water sample. Five types of microplastics, namely polyethylene, polypropylene, acrylonitrile butadiene styrene, acrylonitrile butadiene rubber and polyethylene terephthalate, among which polyethylene is the main type (97 µg/l), were identified. The proposed method is promising for estimation of microplastic content in natural waters.

Zhurnal Analiticheskoi Khimii. 2025;80(3):254-266
pages 254-266 views

Equilibrium and kinetic studies of silver(I) preconcentration on R-modified SMAC sorbent

Afandiyeva N., Maharramov A., Chiragov F.

Аннотация

A new synthetic sorbent (S1) was obtained based on a copolymer of styrene with maleic anhydride and norsulfazole (S) with subsequent modification by the reagent 4,4'-(ethane-1,2-diylbis(azanylidene))bis(pentan-2-one). The structure of the sorbent S was studied by IR and UV spectrometry. The sorption of Ag(I) ions on the sorbents S and S1 was studied. The influence of various parameters on the sorption process was studied, i.e., pH, contact time, and initial concentration of the metal ion. The results of the conducted studies were presented by various models of adsorption isotherms and kinetic models. According to the results of the studies, sorption is best characterized by the Langmuir model and the pseudo-second-order kinetic model. The maximum static sorption capacity was 420.08 mg/g for sorbent S and 577.24 mg/g for sorbent S1. For adsorption studies, a solution of Ag(I) of a concentration of 2 × 10–3 M was used in the work. Static sorption studies were carried out at room temperature. At the final stage, the process of the desorption of the absorbed silver ions was carried out. For this purpose, mineral (HNO3) and organic (CH3COOH) acids were used in the concentration range 0.5–2.0 M. Synthetic sorbents S and S1 were used to extract silver(I) from mushrooms. The results have shown that the modification of the chelating adsorbent with the reagent 4,4'-(ethane-1,2-diylbis(azanylidene))bis(pentan-2-one) was accompanied by an increase in the sorption capacity, i.e., a simultaneous increase in the efficiency of Ag(I) ion extraction by the obtained synthetic sorption material. Comparative characteristics of the maximum adsorption capacities qmax of various adsorbents with respect to Ag(I) showed that the adsorbents S and S1 have higher sorption capacity.

Zhurnal Analiticheskoi Khimii. 2025;80(3):267-278
pages 267-278 views

Determination of volatile components in various extracts from wild chamomile (Matricaria chamomilla L.) flowers by gas chromatographic-mass spectrometry

Temerdashev Z., Chubukina T., Kiseleva N.

Аннотация

The work is devoted to the evaluation of the efficiency of the extraction of volatile organic compounds from flowers of wild chamomile (Matricaria chamomilla L.). The chromatographic-mass spectrometric determination of volatile organic compounds (VOCs) in extracts of wild chamomile flowers extracted by Ginsberg hydrodistillation, liquid-liquid extraction and dispersive liquid-liquid microextraction, as well as extraction under subcritical conditions and ultrasonic (US) treatment was carried out. Volatile compounds were identified by comparing the obtained mass spectra of the components with data from the NIST07 and WILEY8 databases. The contents of analytes in the extracts were estimated by internal normalization of peak areas and by the method of internal standard, as which thujone in acetone was used. VOC contents in essential oil and aromatic water obtained by Ginsberg hydrodistillation, under subcritical conditions and by ultrasonic treatment of acetone extracts from wild chamomile flowers were determined. As macrocomponents of the essential oil, β-Farnesene, α-bisabolol oxide B and bisabolol oxide A were identified. As macrocomponents of the hexane extract from aromatic water, α-Bisabolol oxide B, α-Limonene diepoxide, and bisabolol oxide A were identified. The main component of acetone extracts from wild chamomile flowers obtained under subcritical conditions and ultrasonic treatment was en-in-dicycloether. It was shown that the aromatic water of wild chamomile has higher content and wider list of VOCs in comparison with the essential oil.

Zhurnal Analiticheskoi Khimii. 2025;80(3):267-278
pages 267-278 views

Study of the effect of x-ray radiation on the structural characteristics of bovine serum albumin protein using high-resolution liquid chromatography-mass spectrometry

Brown A., Bliznyuk U., Borshchegovskaya P., Ipatova V., Chernyaev A., Ananyeva I., Rodin I.

Аннотация

A method for assessing changes in the structural characteristics of bovine serum albumin (BSA) protein in aqueous solution as a result of exposure to ionizing radiation has been developed and tested. The method consists of identifying unique peptides of the protein domain structures, as well as establishing amino acid sequence modifications using high-resolution liquid chromatography-mass spectrometry. The BSA solution was irradiated with X-ray radiation with a tube voltage of 80 kV and an average current of 1 mA, the dose rate was 2 Gy/sec. The absorbed dose in the sample volume was estimated by the ferrosulfate dosimetry method. Aqueous solution of BSA was irradiated at doses of 0.1, 0.5, 1, 2, 4, and 8 kGy, after which the content of protein molecules in the solution was quantitatively assessed and the structural integrity of the native form of protein was analyzed, as well as the modifications of amino acids in the BSA sequence as a result of the radiation action were determined. For more in-depth analysis, the reduction of cysteine-cysteine disulfide bonds by BSA followed by alkylation of the resulting thiol residues with bromoacetic acid amide was performed. Enzymatic hydrolysis of BSA was carried out with the addition of trypsin solution. The obtained samples were analyzed by high-resolution liquid chromatography-mass spectrometry with high-resolution tandem mass spectrometric detection. Next, we evaluated the change in the number of intact protein molecules by detecting unique peptides corresponding to each of the three domains that make up the amino acid sequence of BSA. The detection limit of each peptide was calculated taking into account the optimization of conditions for detection of the three domains as markers of the active form of BSA. The developed approach made it possible to determine the change in the natural conformation of bovine serum albumin protein (its denaturation) in aqueous samples as a result of ionizing radiation exposure at doses of 4-8 kGy at an average power of 2 Gy/sec.

Zhurnal Analiticheskoi Khimii. 2025;80(3):279-292
pages 279-292 views

Approximation of the results of gas chromatographic analysis of thermally unstable compounds using logistic regression

Zenkevich I., Kornilova T.

Аннотация

Decomposition of thermally unstable analytes in the chromatograph injector is not uncommon in the practice of gas chromatographic analysis. However, as a rule, it cannot be detected by variations in the absolute areas of gas chromatographic peaks at different injector temperatures. This is hindered by the effects of area discrimination typical of sample dosing into capillary columns with flow division. The problem can be solved using relative peak areas calculated with respect to thermally stable compounds. Dependences of relative peak areas of unstable analytes on temperature (decreasing), as well as of their degradation products (increasing), are characterized by the presence of two limits. The low-temperature limits correspond to the real contents of unstable compounds or their degradation products in samples, and the high-temperature limits correspond to the composition of samples at hypothetically complete transformation of such analytes. Such dependences can be approximated by the logistic regression equation (otherwise – sigmoidal approximation or Boltzmann approximation). To test the applicability of logistic regression for processing the results of gas chromatographic analysis of thermally unstable compounds, the possibilities of approximating the temperature dependence of the peak areas of ethyldiazoacetate in various solvents were analyzed in the present work. The results confirm that gas chromatographic analysis of this ester and, apparently, of other diazocarbonyl compounds without their appreciable decomposition is possible at injector temperatures up to 200°C. The thermal destruction of ethyldiazoacetate in its solutions in aliphatic alcohols is accompanied by the formation of ethyl esters of alkoxyacetic acids – products of the introduction of intermediately formed ethoxycarbonylcarbene into the O–H bonds of alcohols. Such a characteristic of logistic regression as the value of the argument corresponding to the average value of the function indicates that the half-life temperatures of the initial analyte and “half-formation” of the products are the same, which makes it possible to correlate these processes with each other. A slight modification of the proposed method (addition of a point corresponding to the zero peak area at a hypothetical high injector temperature) makes it possible to extend it to characterize compounds with half-life temperatures higher than 300°C. Such a variant was used to test the thermal stability/instability of halogen derivatives of alkyl- and cycloalkylaromatic hydrocarbons under conditions of gas chromatographic analysis.

Zhurnal Analiticheskoi Khimii. 2025;80(3):307-322
pages 307-322 views

Gold nanoparticles electrochemically deposited on carbon nanomaterials and thiacalixarenes in immunosensors for determining tricyclic antidepressants

Brusnitsyn D., Ramazanova A., Medyantseva E., Ramazanova E., Prytkova A., Karimova E., Ziganshin M., Burilov V., Makarov E., Khamidullin T.

Аннотация

Composite materials based on electrochemically deposited gold nanoparticles obtained by cyclic voltammetry and chronoamperometry on a carbon substrate of functionalized graphene oxide, reduced graphene oxide and carbon nanotube paper have been proposed. Composite materials were screened by atomic force microscopy, electrochemical impedance spectroscopy and voltammetry, which allowed us to select the best ones as modifiers of planar electrodes, on the basis of which highly sensitive immunosensors were developed. For the best amperometric immunosensors based on a combination of carbon paper, amino(thia)calix[4]arene, and gold nanoparticles for the determination of amitriptyline and desipramine, the working concentration range was 1 × 10–9–1 × 10–4 M, and the lower limit of detectable concentrations was (4–6) × 10–10 М. Amitriptyline and desipramine were determined by amperometric immunosensors in pharmaceutical preparations with relative standard deviation not exceeding 0.040. Comparison of the results of determination of tricyclic antidepressants by immunosensors and fluorescence polarization immunoassay in human urine with relative standard deviation not exceeding 0.085 indicates the correctness and convergence of the obtained results.

Zhurnal Analiticheskoi Khimii. 2025;80(3):323-336
pages 323-336 views