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卷 80, 编号 7 (2025)
ORIGINAL ARTICLES
Determination of quercetin in pharmaceuticals by digital colorimetry using assemblable microfluidic systems based on paper modified with gold and silver nanoparticles
摘要
One of the actual fields of application of paper-based microfluidic systems (µPADs) is the determination of biologically active substances in various objects, including pharmaceuticals. Often such determination is carried out as a variant of screening analysis to identify samples that should be investigated in more detail by highly informative but relatively expensive methods. In this work, an original method for the colorometric determination of quercetin using microfluidic analytical systems based on paper modified with gold and silver nanoparticles of different morphologies is proposed. It is based on the reduction of silver(I) ions to metallic silver under the action of quercetin, which leads to a contrast color change of the BMFS detection zones. The possibility of using a monitor calibrator and a smartphone camera to record the analytical signal was demonstrated. Optimal conditions of the analysis have been selected. It is shown that the type of nanoparticles affects the sensitivity coefficient of quercetin detection, which is promising for the creation of multisensor systems for discrimination of samples of complex composition. The limits of quercetin detection under the selected conditions are 70-120 ng depending on the nature of the analytical reagent and the method of analytical signal registration. The range of detectable contents is 2-10 µg. Sufficient sample volume for analysis does not exceed 25 µl. The selectivity of the proposed method for the determination of quercetin in relation to a series of common inorganic ions and organic substances was evaluated. The applicability of the developed approach for the determination of quercetin in three pharmaceutical preparations is shown.
Zhurnal Analiticheskoi Khimii. 2025;80(7):641-655
641-655
Identification of species affiliation and determination of fish eggs adulteration by vibrational spectroscopy and digital colorimetry methods
摘要
The efficiency of combining spectroscopic and chemometric methods for identification and classification of salmon, sturgeon and particle fish caviar, as well as for differentiation of natural and imitated samples, has been shown. Analysis of infrared spectra in the near and middle regions made it possible to identify the peculiarities of chemical composition and structure of the samples under study, providing reliable differentiation of natural and imitated caviar. The use of Raman spectroscopy helped to identify characteristic spectral differences related to protein-lipid composition and the presence of carotenoids, which allowed to clearly differentiate the samples. The application of principal component analysis (PCA), hierarchical cluster analysis (HCA) and formal independent modeling of class analogies (SIMCA) algorithms improved classification accuracy, providing separation of samples by fish species. Digital colorometry based on the analysis of optical characteristics in the UV and IR ranges showed to be an affordable and reliable method that can be an alternative to more expensive spectroscopic approaches.
Zhurnal Analiticheskoi Khimii. 2025;80(7):656-671
656-671
Sample preparation of large mass black shale samples using ammonium bifluoride for instrumental analysis by ms/aes-icp methods
摘要
The technique of acid decomposition of 1000 mg black shale samples in an open system has been developed. The procedure involves the destruction of the mineral matrix with a fivefold excess of ammonium bifluoride at 230°C for 6 h, followed by the reagent removal through distillation and the subsequent treatment of the residue with a mixture of perchloric and nitric acids to achieve the complete dissolution. The resulting solution remains stable over time and serves as the basis for the direct determination of more than 60 elements using a combination of ICP–MS and ICP–AES techniques. The method enables the quantification of gold, silver, and rhodium directly in the post-decomposition solution with the computational correction of spectral interferences. The method was tested on reference black shale materials from the Baikal–Vitim province SLg-1 and SChS-1 (Sukhoi Log deposit, Irkutsk region, Russia). The study also presents analytical results for their updated counterparts, SLg-1A and SChS-1A.
Zhurnal Analiticheskoi Khimii. 2025;80(7):672-687
672-687
Gas chromatographic analysis of the content of the organochlorine pesticide lindane in some samples of agricultural products under primary and secondary cultivation in the same soil
摘要
Residual content of the organochlorine pesticide lindane in model samples of tomatoes, cucumbers and onions was investigated by gas chromatography. A solution of the pesticide was added to the soil, after which the data were grown twice in contaminated soil. Two methods of sample preparation were used in the analysis: according to GOST 30349 and similar sample preparation using liquid nitrogen at the stage of homogenization. It was found that the use of liquid nitrogen in sample preparation increases the degree of analyte extraction up to two times. For tomato and cucumber samples, it was found that for both primary and secondary cultivation, the residual amount of organochlorine pesticide increased with increasing concentration of pesticide at spraying. However, this is not characteristic of onion samples. In the latter case, lindane residues decrease with increasing concentration of the parent analyte. This behavior is characteristic of root crop samples, to which onions are not related. The residual content of lindane in different parts of tomato and cucumber plants differs: tomato accumulates the pesticide to a greater extent in the fruit and cucumber in the haulm. In secondary cultivation in contaminated soil, the residual amount of lindane did not exceed 12 % of the original amount. As a result, it was found that the most suitable plant for growing on lindane-contaminated soils is cucumber, as 80-90 % of lindane is accumulated in inedible roots of cucumber, and the fruit contains the least amount of the contaminant among all vegetables. Tomato is unsuitable for cultivation on contaminated soils, as the fruit accumulates a significant amount of lindane.
Zhurnal Analiticheskoi Khimii. 2025;80(7):688-698
688-698
Determination of residual amounts of beta-adrenostimulants in muscle tissue and liver by dispersion purification chromatography-mass spectrometry
摘要
A selective technique for the determination of 20 beta-adrenostimulants in muscle tissue and liver by chromatography-mass spectrometry has been developed. The limit of quantitative determination of the technique is 0.1-0.25 (0.5) µg/kg (depending on the compound to be determined). The technique is based on hydrolysis of research objects followed by extraction of the determined compounds with acetic acid acetonitrile, obtaining the organic fraction by salting, its purification on aluminum oxide layer and dispersive purification with C18, further purification by liquid-liquid extraction with hexane. Data on promising ion-transitions of some determined compounds are given; detection parameters of bambuterol, formoterol, phenylethanolamine A are established. Data on optimization of hydrolysis, extraction and purification of extracts are given. Information on stage-by-stage losses of the determined compounds is given; data on the analysis of reference material are obtained. The validation of the developed method shows that the relative expanded uncertainty ranges from 7 to 24 %.
Zhurnal Analiticheskoi Khimii. 2025;80(7):699-711
699-711
HPLC-MS/MS-determination of antihistamines cyproheptadine, diphenhydramine and tripelenamine in foods and feeds
摘要
The method of determination of antihistamine substances cyproheptadine, diphenhydramine and tripelenamine in food and feed by high-performance liquid chromatography-tandem mass spectrometry was proposed. When developing the method, its versatility in terms of reagents and equipment used in the analysis of matrices of different types – meat, offal (liver), eggs, milk, honey, butter, as well as mixed fodder – was considered as the main aspect. A combination of solvents was used for the isolation of analytes: acetonitrile, water and hexane (3 ml of each), the sequence of solvent addition depended on the matrix, the rest of the sample preparation steps were unified. The limits of detection and determination of antihistamines in the above objects were 0.012-0.3 and 0.04-1 μg/kg, respectively. The relative standard deviation of the analytical results does not exceed 17 %. The relative error of determination of substances in most cases does not exceed 15 %.
Zhurnal Analiticheskoi Khimii. 2025;80(7):712-721
712-721
Voltammetric sensor based on tin dioxide nanoparticles for the determination of taxifolin
摘要
A voltammetric sensor based on a glassy carbon electrode (GCE) modified with tin dioxide nanoparticles dispersed in N-hexadecylpyridinium bromide (NPs SnO2) was developed for the determination of taxifolin. Modification of the electrode surface provides an increase in the reversibility of the electrode reaction, as well as a significant increase in the redox currents compared to GCE (2.3 and 3.3 times for the anodic and cathodic peaks, respectively). The morphology of the electrode surface according to scanning electron microscopy data is represented by uniformly distributed on the electrode surface SnO2 NPs of spherical shape with a diameter of 20-40 nm, which leads to a 3.9-fold increase in the effective area of the electrode and a 143-fold increase in the heterogeneous electron transfer rate constant. The electrooxidation of taxifolin was found to proceed with the participation of protons. Mixed control with diffusion and adsorption contributions was confirmed for the electrode reaction. In differential pulse mode against Britton-Robinson buffer with pH 6.0, the range of determined taxifolin contents is 0.075-25 μM with a detection limit of 70.7 nM. The obtained characteristics are comparable to other electrochemical approaches, but the proposed approach is simpler and more rapid, and does not require complex modification of the electrode. The developed sensor was successfully applied in the analysis of dihydroquercetin (taxifolin) based bioadditives. The results obtained were compared with the data of coulometric titration by electrogenerated bromine.
Zhurnal Analiticheskoi Khimii. 2025;80(7):722-733
722-733
High-resolution voltammetric determination of carmoisine, Allura Red and Brilliant Blue on their simultaneous presence in food products
摘要
A voltammetric sensor is developed based on a carbon fiber planar electrode modified with a nanocomposite for the simultaneous determination of the synthetic food dyes carmoisine (Car), allura red (AR), and brilliant blue (BB). The nanocomposite includes nickel oxide nanoparticles synthesized using a strawberry leaf extract, graphene nanoplates and the cationic surfactant cetyltrimethylammonium bromide. The modified electrode exhibits enhanced signal responses for all three colorants at an improved resolution. Electrochemical oxidation proceeds irreversibly, governed by surface-controlled processes in the cases of Car and BB, and by diffusion-controlled processes in the case of AR. The proposed method enables the simultaneous voltammetric determination of Car, AR, and BB using the developed sensor. The limits of detection for Car, AR and BB are 0.05, 0.08 and 0.15 μM, respectively. Under the selected conditions for recording differential pulse voltammetry signals, real samples including soft drinks, syrup, and marshmallows were successfully analyzed, yielding accuracy values ranging from 95 to 104%.
Zhurnal Analiticheskoi Khimii. 2025;80(7):734-744
734-744
New micellar polymers as polyfunctional modifiers of electrophoretic systems
摘要
New modifiers of electrophoretic systems – cationic polyelectrolytes with micellar properties poly-11-acryloyloyloxyundecyl-N-methylpiperidinium bromide (pAUMP-Br), poly-11-acryloyloxyundecylpyridinium bromide, poly-11-acryloyloxyundecyl-1,4-diazobicyclo[2. 2.2.2.2]octan-1-ium bromide and a chiral copolymer based on acylated quinine and N-(11-acryloyloyloyloxyundecyl)-N-methylpiperidinium bromide (pAUMP-AQin). The electrophoretic capabilities of these polymers were studied in the separation of model mixtures of biologically active substances: steroid hormones, biogenic amines and amino acids in the modes of micellar electrokinetic chromatography and capillary electrochromatography. It was found that new polyelectrolytes are polyfunctional modifiers of quartz capillary walls and background electrolyte and allow to realize different modes of electrophoretic separation of biologically active substances, indirect detection in the presence of chromophoric group in the polymer composition, generate anodic electroosmotic flow, influence the efficiency and selectivity of analytes separation. Field-amplified sample stacking was performed on a quartz capillary modified with pAUMP-Br, providing a 15-fold concentration of biogenic amines and lowering the detection limits. The chiral labeled pAUMP-AQin copolymer was found to facilitate the separation of tryptophan enantiomers.
Zhurnal Analiticheskoi Khimii. 2025;80(7):745-755
745-755
CRITIQUE AND BIBLIOGRAPHY
НОВЫЕ КНИГИ ИЗДАТЕЛЬСТВ ELSEVIER И ACADEMIC PRESS
Zhurnal Analiticheskoi Khimii. 2025;80(7):756-756
756-756