Journal of Analytical Chemistry最新文献

{"title":"Determination of Polychlorinated Biphenyls in Aquatic Organisms as Pollution Bioindicators at Ultratrace Concentration Levels","authors":"O. V. Kustova,&nbsp;A. G. Gorshkov","doi":"10.1134/S1061934826700176","DOIUrl":"10.1134/S1061934826700176","url":null,"abstract":"<p>A procedure for the determination of indicator congeners of polychlorinated biphenyls (PCBs) in the aquatic organisms of Lake Baikal, an aquatic ecosystem characterized by trace levels of pollutants in water, has been validated. The procedure included ultrasonic extraction of analytes from samples weighing up to 0.5 g and purification of the extracts with sulfuric acid. Gas chromatography–mass spectrometric analysis with detection of analytical peaks in the multiple reaction monitoring mode and the use of ¹³C-labeled surrogate internal standards ensured the determination in a range of 0.10 to 15 ng/g with an accuracy of ±δ = 24–28% (<i>P</i> = 0.95) and, for congener no. 180, in a range of 0.010 to 15 ng/g with an accuracy of ±δ = 45%. The composition and accumulation level of PCBs, including indicator and dioxin-like congeners, were determined in the Baikal fish species <i>Coregonus migratorius</i> (Georgi, 1775), <i>Comephorus baicalensis</i> (Pallas, 1776), and <i>Comephorus dybowskii</i> (Korotneff, 1904) and in the mollusks <i>Benedictia baiсalensis</i> (Gerstfeldt, 1859) and <i>Radix auricularia</i> (Linnaeus, 1758). The studied aquatic organisms were evaluated as sensitive indicators of ultratrace amounts of PCBs in the water of Lake Baikal.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"581 - 591"},"PeriodicalIF":1.1,"publicationDate":"2026-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147808263","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determination of Cinnamaldehyde in Cinnamon Essential Oil Based on Iodometry Using Bisulfite","authors":"Zhuo Chen,&nbsp;Nan Li","doi":"10.1134/S1061934826700206","DOIUrl":"10.1134/S1061934826700206","url":null,"abstract":"<p>Based on the nucleophilic addition reaction between cinnamaldehyde and bisulfite, this study develops an analytical method for determining the cinnamaldehyde content in cinnamon essential oil using iodometric back-titration. Cinnamaldehyde reacts quantitatively with excess bisulfite, and the unreacted bisulfite is titrated with iodine. The method demonstrated a strong linear relationship (<i>R</i>² = 0.9999) within the concentration range of 2–15 mg/mL, with a detection limit of 0.32 mg/mL and a quantification limit of 1.07 mg/mL. Recovery tests using Chinese and Ceylon cinnamon essential oils showed recovery rates between 96.0 and 99.4%, with intra-day and inter-day relative standard deviations below 2%. The results were consistent with those obtained by gas chromatography. The method is accurate, reproducible, and cost-effective, and does not require sophisticated instrumentation, making it widely applicable for quality control and authenticity assessment of cinnamon essential oils. This work provides a low-cost and reliable method for the determination of cinnamaldehyde in cinnamon essential oil.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"628 - 633"},"PeriodicalIF":1.1,"publicationDate":"2026-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147808203","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Synergistic Integration of Reduced Graphene Oxide and Molecularly Imprinted Polymer on an Interdigital Electrode for Real-Time and Ultra-Trace Detection of Melamine","authors":"Samra Ashraf,&nbsp;Ghulam Mustafa,&nbsp;Khalid Pervaiz,&nbsp;Mubushar Majeed","doi":"10.1134/S1061934825603482","DOIUrl":"10.1134/S1061934825603482","url":null,"abstract":"<p>Melamine (<b>MEL</b>), a nitrogen-rich compound illicitly added to milk and dairy products to falsify protein content, poses severe health hazards, including nephrotoxicity, renal failure, and infant mortality. In this study, a rationally designed reduced graphene oxide-poly(methacrylic acid-co-ethylene glycol dimethacrylate) hybrid film immobilized on an interdigital electrode is presented for the development of a high-sensitivity electrochemical sensor for MEL detection. Density functional theory calculations identified methacrylic acid as the most favorable functional monomer and dimethyl sulfoxide as the optimal porogenic solvent, ensuring stable pre-polymerization complex formation with MEL. The successful synthesis of the imprinted matrix and complete template removal were confirmed by Fourier-transform infrared spectroscopy and ultraviolet–visible spectroscopy, respectively, while surface morphology was characterized using scanning electron microscopy and atomic force microscopy, revealing a porous and uniformly imprinted topology. The fabricated reduced graphene oxide (<b>rGO</b>)-molecularly imprinted polymer (<b>MIP</b>)-based interdigital electrode sensor exhibited an excellent linear sensor response toward MEL concentrations ranging from 1 to 90 ppm (<i>R</i>² = 0.9908), achieving a limit of detection of 30 ppb and a limit of quantification of 129 ppb, outperforming conventional MIP sensors by nearly an order of magnitude. The synergistic combination of rGO and MIP significantly enhanced electron transfer kinetics and binding-site accessibility, resulting in superior sensitivity, selectivity, and stability compared to non-imprinted controls. The sensor demonstrated remarkable reproducibility (relative standard deviation &lt;3%), reusability, and long-term stability, underscoring its potential for rapid, on-site, and real-time monitoring of MEL contamination in complex food matrices.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"693 - 707"},"PeriodicalIF":1.1,"publicationDate":"2026-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147808219","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Improving the Performance of an Adsorptive Membrane by Modifying Attapulgite and Its Application to the Detection of Chlorophenols","authors":"Yinuo Huang,&nbsp;Shuaibin Wu","doi":"10.1134/S1061934826700243","DOIUrl":"10.1134/S1061934826700243","url":null,"abstract":"<p>In this study, the surface covalent reaction method was adopted to modify attapulgite on the surface of polypropylene adsorption membranes for the adsorption of small molecular compounds. Compared with various materials currently modified on the surface of polypropylene adsorption membranes, attapulgite has the characteristics of low cost and environmental friendliness, which is more conducive to large-scale practical application. The prepared polypropylene adsorption membrane modified with attapulgite was characterized by field emission scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray diffractometry, etc. The experimental results showed that attapulgite was successfully modified on the surface of the polypropylene adsorption membrane. The subsequent adsorption experiment results indicated that within 1 min, the adsorption capacities of chlorophenol and Congo red by the polypropylene adsorption film modified with attapulgite could reach 6 and 3 mg/g, respectively; the minimum detectable concentration could reach 0.02 mg/mL, with a relative standard deviation of about 12.7%.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"664 - 671"},"PeriodicalIF":1.1,"publicationDate":"2026-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147808264","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determination of Persistent Organic Pollutants in Surface Waters at Trace Concentration Levels: Challenges and Solutions","authors":"A. G. Gorshkov,&nbsp;T. A. Grigoryeva,&nbsp;O. V. Kustova","doi":"10.1134/S1061934826700164","DOIUrl":"10.1134/S1061934826700164","url":null,"abstract":"<p>Methods for the determination of polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs), and phthalic acid diesters (phthalates) in surface waters at trace concentration levels are considered. Lake Baikal, whose waters are characterized by trace levels of pollutants, was selected as a natural model for the study. The methods are combined into an analytical procedure including the collection of 1-L water samples, liquid–liquid extraction with <i>n</i>-hexane, preconcentration of the extracts, and analysis by gas chromatography–mass spectrometry. The accuracy indicator (±δ) for the determination of PCBs at concentrations from 0.02 to 0.90 ng/L ranges from 10 to 35%; for PAHs at concentrations from 0.10 to 15 ng/L, from 8.0 to 35%; and for phthalates at concentrations from 0.01 to 0.66 μg/L, from 12 to 38%. An online method for the determination of dominant phthalates in water by high-performance liquid chromatography has been validated, which reduces the risk of contamination of samples by background phthalates: sample volume 4 mL, concentration range 0.14–6.0 μg/L, and determination error 15–20%.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"571 - 580"},"PeriodicalIF":1.1,"publicationDate":"2026-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147808266","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Spectral Curves and Light Absorption Indices as Indicators of Changes in the Genesis of Chromophoric Dissolved Organic Matter in Natural Water Bodies of the Russian North (A Case Study of Lake Imandra)","authors":"M. M. Bazova,&nbsp;S. S. Solovieva","doi":"10.1134/S1061934826700127","DOIUrl":"10.1134/S1061934826700127","url":null,"abstract":"<p>This study evaluates the potential of spectral characteristics of dissolved organic matter (DOM) as indicators of changes in the dominant type of chromophoric dissolved organic matter in Lake Imandra, including variations in the balance between allochthonous and autochthonous organic matter and the degree of humification of natural waters under the influence of anthropogenic and natural processes in the reservoir. Absorption and fluorescence spectroscopy were used to obtain the spectral characteristics of DOM. The relationships between spectral indices and bulk concentrations of organic carbon, nutrients, and heavy metals were analyzed. Particular attention was given to the effect of anthropogenic sulfate inputs on the light-absorption properties of DOM in surface and near-bottom water layers of the lake. In addition, relationships between water color, humification indices, and the relative contribution of allochthonous and autochthonous organic matter were examined. Although this approach is still relatively underutilized, it allows the degree of humification and the ratio between high-molecular-weight allochthonous humic substances transported from the catchment area and low-molecular-weight compounds formed within the reservoir during production–decomposition processes to be determined with high accuracy.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"531 - 539"},"PeriodicalIF":1.1,"publicationDate":"2026-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147808201","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determination of Trace Quantities of Iron in Natural Substances with 3-(3'-Hydroxy-4'-Carboxyphenylazo)Pentadione-2,4 and Diantypyrylmethane and its Homologues","authors":"Khalil Nagiev,&nbsp;Ul’viya Gyullyarli,&nbsp;Arzu Abieva,&nbsp;Famil’ Chyragov","doi":"10.1134/S106193482670022X","DOIUrl":"10.1134/S106193482670022X","url":null,"abstract":"<p>The complexation of iron(III) with 3-(3'-hydroxy-4-carboxyphenylazo)pentadione-2,4 (<b>R</b>) in the presence of diantipyrylmethane (<b>DAM</b>) and its homologues, diantipyrylpropylmethane (<b>DAPM</b>) and diantipyrylphenylmethane (<b>DAPhM</b>), is studied, and selective spectrophotometric procedures for determining its trace amounts in complex natural samples are developed. In an acidic medium, iron(III) with reagent R in the presence of diantipyrylmethane and its homologues forms mixed-ligand complexes Fe(III)-R-DAM, Fe(III)-R-DAPM and Fe(III)-R-DAPhM with a component ratio of 1 : 1 : 1, while bathochromic shifts and hyperchromic effects are observed in the absorption spectra, as well as a shift of the yield maximum to a more acidic medium compared to the homogeneous-ligand complex Fe(III)-R. The yield of the Fe(III)-R-DAM complex is maximum at pH 1.5–2.0, and of the Fe(III)-R-DAPM and Fe(III)-R-DAPhM complexes at pH 2.0–2.5. The influence of the concentration of reactants, temperature and time on the formation of the complexes is studied. The stability constants of the complexes are determined and it is found that in the presence of diantipyrylmethane and its homologues, the stability of the complexes increases by more than three orders of magnitude. Astakhov’s method is used to elucidate the chemistry of the formation of homogeneous and mixed-ligand iron(III) complexes. The calibration curves for determining iron(III) as homogeneous and mixed-ligand complexes are linear. A study of the effect of foreign ions on the determination of iron(III) revealed that the presence of diantipyrylmethane and its homologues significantly increases the selectivity of the reaction. The determination of iron(III) in the form of mixed-ligand complexes Fe(III)-R-DAM, Fe(III)-R-DAPM, and Fe(III)-R-DAPhM is not interfered with by more than 1000-fold amounts of Ca(II), Ba(II), Mg(II), Co(II), Ni(II), Zn(II), Mn(II), Cd(II), and other ions. The developed procedures are tested in the determination of trace amounts of iron in champignon mushrooms grown in the village of Zire, Baku, in cherries, and in water sampled from the Caspian Sea near the village of Turkan, Baku.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"651 - 656"},"PeriodicalIF":1.1,"publicationDate":"2026-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147808218","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Antibody-Based Monitoring of Nitroaromatic Explosive Contaminants in the Environment","authors":"Nevena Zelenović,&nbsp;Mladen Simonović,&nbsp;Milica Popović","doi":"10.1134/S1061934825602427","DOIUrl":"10.1134/S1061934825602427","url":null,"abstract":"<p>Nitroaromatic compounds (<b>NAC</b>s), which are frequently used as explosives, represent a class of persistent xenobiotics with considerable biochemical and ecological relevance. Their detection in complex matrices such as soil and water represents a major analytical challenge. Although chromatographic and mass spectrometric methods offer high sensitivity, their applicability is limited by demanding sample preparation and instrumentation. In recent years, immunochemical methods have established themselves as highly selective bioanalytical tools for the detection of trace amounts of NACs. This review highlights the structural principles of hapten-antibody interactions, the production and characterization of monoclonal and recombinant antibodies, and their application in immunoassays and lateral flow devices. A particular focus is placed on the development of antibody fragments and nanobodies that offer improved thermal and chemical stability, reduced steric hindrance, and compatibility with biosensor technologies. The integration of immunoassay formats with transducer platforms is discussed in the context of the further development of field-ready diagnostics. Immunodetection is thus an example of a bioanalytical strategy that combines molecular detection with biochemical assay design and represents a robust alternative for monitoring environmental pollutants of toxicological concern.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"614 - 627"},"PeriodicalIF":1.1,"publicationDate":"2026-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147808182","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determination of the Impurity Composition of Polyethylene Terephthalate, Polypropylene, and Expanded Polystyrene by Inductively Coupled Plasma Atomic Emission and Mass Spectrometry","authors":"T. Ya. Guselnikova,&nbsp;A. R. Tsygankova,&nbsp;N. A. Orlov","doi":"10.1134/S1061934825701679","DOIUrl":"10.1134/S1061934825701679","url":null,"abstract":"<p>The paper presents procedures for the determination of a wide range of elements in polyethylene terephthalate (<b>PET</b>), polypropylene (<b>PP</b>), and expanded polystyrene (EPS). It proposes dissolution of PET, PP, and EPS in a mixture of H₂SO₄ and HNO₃ upon heating in open quartz vessels. The resulting solutions are analyzed by inductively coupled plasma atomic emission spectrometry (ICP <b>AES</b>) and inductively coupled plasma mass spectrometry (<b>ICP</b> <b>MS</b>). Optimal (compromise) concentrations of matrix component in the analyzed solutions are determined: 1100 and 700 mg/L for ICP AES and ICP MS, respectively. Y and Be are used as internal standards for ICP AES analyses. For the ICP MS analysis, an internal standard (Rh) is required to determine B, Bi, Ni, and Sc. The developed procedures enable the determination of 55 elements by ICP AES with limits of detection (<b>LOD</b>s) ranging from 0.06 to 70 µg/g, and 48 elements by ICP MS with LODs ranging from 0.001 to 10 µg/g. The validity of the developed procedures is confirmed using the spike experiments. Using the developed procedures, concentrations of a total of 32 elements are determined in previously used commercial products; concentrations of the remaining elements are below the LODs of the procedures.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"413 - 423"},"PeriodicalIF":1.1,"publicationDate":"2026-04-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147636910","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Study of the Composition, Size, and Morphology of Solid Aerosols in Workplace Air","authors":"A. R. Tsygankova,&nbsp;T. Ya. Guselnikova,&nbsp;A. I. Saprykin,&nbsp;M. O. Firsov,&nbsp;A. V. Volzhenin,&nbsp;M. A. Zenkova,&nbsp;E. B. Logashenko,&nbsp;A. V. Senkova,&nbsp;I. A. Savin","doi":"10.1134/S1061934825701722","DOIUrl":"10.1134/S1061934825701722","url":null,"abstract":"<p>The article reports a physicochemical study of the composition, size, and morphology of solid aerosol particles of industrial origin, specifically particles collected from the air of working zones at a forging press, sandblasting and grinding sections, and a blast furnace. Particles were collected from workplace air by absorption in deionized water. Scanning electron microscopy enabled an analysis of sample morphology and local particle size. The results demonstrate the feasibility of using atomic force microscopy, previously not used to characterize the particle size distribution of solid aerosols. Energy-dispersive spectrometry established the matrix elemental composition of individual particles, including Al, Cr, Cu, Fe, S, Sn, W, Zn, and Zr. The detected solid particles ranged in size from 0.3 to 20 μm, and their composition corresponded to the steels, alloys, and materials being processed and used for treatment. Inductively coupled plasma atomic emission spectrometry determined the bulk composition of the aerosol solid particles, which contained Al, B, Ba, Ca, Cu, Fe, K, Mg, Mn, Na, Ni, P, S, Si, Sr, and Zn. The concentrations of the identified elements in the workplace air varied from 0.26 to 1.1 × 10⁶ ng/L of air. For Ca, Na, P, S, and Si, the concentrations exceeded the maximum permissible concentration by factors of 1.5 to 100.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"474 - 481"},"PeriodicalIF":1.1,"publicationDate":"2026-04-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147636915","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}