Zhurnal Analiticheskoi Khimii

ISSN (print): 0044-4502

Media registration certificate: No. 0110234 dated 02/09/1993

Founder: Institute of Geochemistry and Analytical Chemistry named after. V.I. Vernadsky RAS, Russian Academy of Sciences

Editor-in-Chief: Kolotov, Vladimir Panteleimonovich

Number of issues per year: 12

Indexation: RISC, list of Higher Attestation Commissions, CrossRef, White List (level 3)

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卷 80, 编号 10 (2025)

年: 2025
文章: 11
URL: https://journals.rcsi.science/0044-4502/issue/view/21419

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REVIEWS

Chemometrics for optical spectral analysis of multicomponent mixtures

Bogomolov A., Manankov A.

摘要

Modern optical spectroscopy effectively solves the problems of quantitative and qualitative analysis of multicomponent mixtures with complex chemical and morphological composition. Many natural and man-made samples require direct analysis without separation into components or complex sample preparation, and often without the possibility of physical sampling. This has become possible thanks to the technical improvement of analytical instruments on one hand, and the development of mathematical methods for analyzing multidimensional data (chemometrics) on the other. This review focuses on the most important chemometric algorithms in terms of their contribution to the creation and advancement of optical spectral methods for analyzing multicomponent mixtures. Emphasis is placed on molecular spectroscopy in the ultraviolet, visible, and infrared regions, where, due to significant overlap of absorption (or emission) bands, the accuracy and robustness of the analysis results heavily depend on the mathematical tools used. The article presents foundational theoretical information that provides insight into the effectiveness of the discussed methods and algorithms in building models for calibration, classification, and exploratory analysis of multidimensional data. Some of the material is presented in Russian-language scientific literature for the first time. Illustrative examples are provided showing the application of optical spectroscopy and chemometrics to solve real-world analytical problems in the chemical, food, and pharmaceutical industries, as well as in environmental and medical fields – without prior sample preparation.

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Zhurnal Analiticheskoi Khimii. 2025;80(10):1007-1030

1007-1030

(Rus)

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The extraction freezing method: twenty years of development

Bekhterev V.

摘要

This article reviews the results of twenty years of development of the extractive freezing-out method. The novel principle of extraction is based on low-temperature isolation of target components via redistribution of dissolved substances between the liquid phase of a pre-added non-freezing hydrophilic solvent and the forming solid phase of ice during freezing. A major advancement in the method was the introduction of extractive freezing-out under the influence of centrifugal forces (EFC). Implementing EFC as a sample preparation step in various methods for determining organic substances has enabled the successful integration of the technique into chemical-toxicological analysis, food quality control, environmental monitoring, and hydrochemical studies. The article demonstrates the advantages of the developed extraction method in comparison with traditional techniques such as liquid–liquid extraction, headspace analysis, and solid-phase extraction. It also outlines the near-term prospects for further development.

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Zhurnal Analiticheskoi Khimii. 2025;80(10):1031-1044

1031-1044

(Rus)

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ORIGINAL ARTICLES

Application of mimetic analogs for the preparation of a bioinorganic sorbent modified with imprinted proteins

Presnyakov K., Ilyicheva P., Tsyupka D., Menyaylo I., Burmistrova N., Pidenko P.

摘要

A method has been developed for obtaining a specific bioinorganic sorbent based on silicon dioxide (IV) particles modified with an imprinted protein (IP). Bovine serum albumin was used as the template protein molecule. The imprinting was carried out in the presence of a series of template molecules – coumarin, 4-hydroxycoumarin, quercetin, and 5,7-dimethoxycoumarin –which act as mimetic analogs of the mycotoxin zearalenone. To preliminarily assess the possibility of substituting zearalenone with mimetic analogs and to select the optimal template molecule concentrations during IP preparation, computational chemistry methods were used (molecular docking and molecular dynamics). The need for prior surface modification of the silicon dioxide (IV) particles to produce sorbents based on IPs was demonstrated. The potential application of the resulting bioinorganic sorbents for solid-phase extraction of template molecules from model solutions was validated for coumarin (Q = 2.0 mg/g), 4-hydroxycoumarin (Q = 1.2 mg/g), quercetin (Q = 0.8 mg/g), 5,7-dimethoxycoumarin (Q = 2.2 mg/g), and for zearalenone (ZEA) from wheat extract (Q = 4.79 mg/g, IF = 2.45). Sorption isotherms were constructed for ZEA on the IP-modified sorbents obtained using different mimetic analogs. Cytotoxicity of the IPs was studied, and biosafety was assessed using the AGREEMIP tool.

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Zhurnal Analiticheskoi Khimii. 2025;80(10):1045-1055

1045-1055

(Rus)

(JATS XML)

Micellar-extraction express determination of certain pharmaceutical arylamines

Sokolova T., Doronin S.

摘要

A method is proposed to lower the detection limit of p-aminobenzoic acid and some of its pharmaceutical derivatives in condensation reactions with p-dimethylaminobenzaldehyde. The approach is based on a combination of anionic catalysis (“micellar catalysis” effect) and preconcentration using nonionic surfactants (“micellar microextraction” effect). The conditions for obtaining micelle-saturated phases of Triton X-114 were optimized both in the absence and presence of sodium dodecyl sulfate (SDS) ions and micelles, reactants, and salting-out agents (NaCl, Na₂SO₄, Na₃C₆H₅O₇). As test media, micelle-saturated phases of Triton X-114 and SDS were proposed, which enable effective concentration of the Schiff base analytical forms of the analytes. These can then be determined at nanogram levels in aqueous solutions, blood plasma models, and pharmaceutical formulations at concentrations of approximately n × 10^–⁸ M using colorimetry methods enhanced by digital technologies.

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Zhurnal Analiticheskoi Khimii. 2025;80(10):1056-1065

1056-1065

(Rus)

(JATS XML)

Study of organic matter distribution on human skin surface using oxithermography

Voloshina E., Zuev B., Mikhailova A.

摘要

An analytical approach is proposed for diagnosing organic matter present on the surface of human skin. This approach combines sampling with the oxithermographic determination method. A quartz rod with a roughened end surface is used as the sampler, which is pressed against the skin area being analyzed. The amount of oxygen consumed in the oxidation of organic matter transferred from the surface of the skin to the sampler is measured. The method does not require the use of chemical reagents since oxidation is performed in an air stream. The detectable range of organic matter, expressed in terms of oxygen, is from 41 to 250 µg O₂/cm². The relative standard deviation ranges from 0.01 to 0.05. The proposed method for assessing the skin condition using the “skin oiliness” indicator may be used for routine monitoring in medical cosmetology, for instance, in acne treatment.

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Zhurnal Analiticheskoi Khimii. 2025;80(10):1066-1071

1066-1071

(Rus)

(JATS XML)

Identification and chromatographic determination of certain functional additives in mineral hydraulic oils

Temerdashev Z., Ivanova Y., Kiseleva N., Chernaya L.

摘要

Methods are proposed for identifying and determining a range of antioxidant, anticorrosion, and dispersing additives–ionol, diphenylamine, zinc dialkyldithiophosphate, and diester oil–in mineral hydraulic oils. The procedure includes preliminary solid-phase extraction of analytes using a cartridge with hydroxylated silica gel, followed by reversed-phase high-performance liquid chromatography detection. Extraction efficiencies exceeded 97%. The limits of detection and quantification for the additives in mineral hydraulic oil were as follows: For ionol: 0.0006% (LOD) and 0.001% (LOQ), for zinc dialkyldithiophosphate: 0.008% and 0.01%, for diphenylamine: 0.00025% and 0.0005%, respectively. It was found that Shell Tellus S2 V 46 hydraulic oil contained 0.16% zinc dialkyldithiophosphate and 0.2% diphenylamine, while Total Hydragri ISO VG 46 contained 0.14% ionol and 0.17% zinc dialkyldithiophosphate. Gel permeation chromatography was used to determine molecular weight characteristics of polymer additives in hydraulic oils, and the viscosity modifier content was calculated for a real sample. The developed methods allow for the detection of functional additives and for the quality control of mineral hydraulic oil.

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Zhurnal Analiticheskoi Khimii. 2025;80(10):1072-1081

1072-1081

(Rus)

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Application of untargeted GC-MS analysis for the identification of cancer biomarkers among steroid hormones in human urine

Gashimova E., Podzhivotov A., Temerdashev A., Malitskaya T., Perunov D., Polyakov I., Porkhanov V.

摘要

The steroid profile is an informative tool both for doping control and clinical diagnostics. Untargeted analysis enables the identification of many compounds that may serve as potential biomarkers of various diseases. In this study, an untargeted GC-MS analysis was conducted on urine samples from 22 cancer patients with different localizations and 22 healthy volunteers. A total of 54 steroid hormones and several fatty acids were identified in the samples. Statistical analysis of the GC-MS data was performed using the Mann–Whitney test and Principal Component Analysis (PCA). Significant differences were found for 46 steroid hormones and 6 fatty acids between the cancer and healthy groups. Projection of the observations onto the factor plane allowed the two groups to be separated, demonstrating the potential of untargeted GC-MS analysis for cancer biomarker discovery.

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Zhurnal Analiticheskoi Khimii. 2025;80(10):1082-1091

1082-1091

(Rus)

(JATS XML)

Application of [(2-hydroxybenzaldehyde)-3-isatin]-bis-hydrazone for photometric determination of palladium(ii) in nickel anode material

Abilova U., Mammadova C., Chyragov F.

摘要

A new complexing analytical reagent was synthesized via the condensation of salicylaldehyde with isatin hydrazone. The dissociation constant of the reagent was determined to be pK = 9.48 ± 0.03. The structure of the reagent was characterized using X-ray diffraction and NMR spectroscopy. Spectrophotometric studies were conducted to investigate the complexation of palladium(II) with [(2-hydroxybenzaldehyde)-3-isatin]-bis-hydrazone (R), both in the presence and absence of third components: diantipyrylmethane (DAM), 8-hydroxyquinoline (8-Ox), and diphenylguanidine (DPG). Optimal complexation conditions (optimal wavelength and pH) were established. It was found that Pd(II) forms colored mixed-ligand complexes with the reagent and these third components. The Pd(II)–R complex showed maximum absorbance at 440 nm, while Pd(II)–R–DAM, Pd(II)–R–8-Ox, and Pd(II)–R–DPG had absorption maxima at 465, 490, and 450 nm, respectively. Molar absorption coefficients were: Pd(II)–R: 6000 L/(mol·cm), Pd(II)–R–DAM: 10,000 L/(mol·cm), Pd(II)–R–8-Ox: 8000 L/(mol·cm), Pd(II)–R–DPG: 7500 L/(mol·cm). The optimal pH values were: Pd(II)–R: pH 4, Pd(II)–R–DAM and Pd(II)–R–DPG: pH 2, Pd(II)–R–8-Ox: pH 3. Stability constants of the complexes were determined. The applicability of Beer's law was established, and calibration equations were obtained via the least squares method. The component ratios in both binary and mixed-ligand complexes were determined using molar ratio, continuous variation (Job’s method), and equilibrium shift methods. All methods showed the following stoichiometries: Pd(II)–R (binary complex): 1 : 2, Pd(II)–R–8-Ox and Pd(II)–R–DPG: 1 : 1 : 1, Pd(II)–R–DAM: 1 : 2 : 1. The effect of various interfering ions and masking agents on complex formation was studied. It was found that Na(I), K(I), Ca(II), Ba(II), Cd(II), Ni(II), Cr(III), Co(II), Pd(IV), platinum group metals, and many anions do not interfere with the determination of Pd(II). The developed method was successfully applied for the determination of trace amounts of palladium(II) in nickel anode material.

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Zhurnal Analiticheskoi Khimii. 2025;80(10):1092-1099

1092-1099

(Rus)

(JATS XML)

Determination of the impurity composition of boric acid by inductively coupled plasma atomic emission spectrometry

Nagornaya S., Polyakova E., Nikolaev R.

摘要

Methodologies were developed for the ICP-AES determination of 53 impurities (including rare earth elements) in boric acid. To select optimal analysis conditions, the signal behavior of impurity elements was studied at boron concentrations of 0–5000 mg/L and plasma powers of 1000, 1300, and 1600 W under axial observation. The maximum analytical signals for most impurity elements were observed at the highest investigated plasma power and the greatest boron content in the solution. Given the significant matrix effect of boron (from ~500 mg/L), calibration curves were constructed using the method of standard additions. The accuracy of the analysis was confirmed using the “added–found” experiment, yielding recovery rates of 85–115%. Detection limits based on the 2s criterion ranged from n × 10^–⁷ to n × 10^–⁴ mass %.

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Zhurnal Analiticheskoi Khimii. 2025;80(10):1100-1107

1100-1107

(Rus)

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Application of Capillary Electrophoresis for the Study of Synthetic Phosphate Degradation in Meat Systems

Tyutyaev E., Maksimov G.

摘要

A capillary electrophoresis (CE) method was developed and implemented for the determination of synthetic polyphosphates (SPs) in meat products (MP). SP content is monitored in filtered extracts of meat samples. Extraction and separation conditions were developed, and suitable capillary geometries and detection parameters for SPs were selected. It was shown that the content of tri- and diphosphates in meat products decreases over time at different rates (triphosphates degrade faster than diphosphates at the same temperature), depending both on storage temperature and technological processes during meat product manufacturing.

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Zhurnal Analiticheskoi Khimii. 2025;80(10):1108-1114

1108-1114