Journal of Analytical Chemistry最新文献

{"title":"Dynamic Role of Scanning Electron Microscopy Coupled with Energy-Dispersive X-ray Spectroscopy in Differentiating Overlapped Blue Pen Inks","authors":"Mandeep Kaur Purba,&nbsp;Shruti Gupta,&nbsp;Reeta Rani Gupta","doi":"10.1134/S1061934824603773","DOIUrl":"10.1134/S1061934824603773","url":null,"abstract":"<p>Documents serve as a testament to societal responsibilities, representing tangible evidence of interactions and agreements among individuals, organizations, and clients. The diversity of their form varies from printed, typewritten, or handwritten materials. This study highlights the dynamic role of scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (<b>SEM-EDX</b>) in differentiating overlapped blue pen inks, providing a valuable tool for forensic document examination. In the present work, elemental analysis was conducted on blank paper, individual inks (B1, B2, G1, G2, F1, F2), and their respective overlap regions (B1B2, G1G2, F1F2) to investigate compositional variations. The overlap regions exhibited intermediate elemental profiles, reflecting contributions from both inks. Elevated carbon levels confirmed the organic composition of inks, while reduced oxygen and magnesium levels indicated ink coverage on the paper surface. Unique elemental markers, such as copper in gel inks, calcium in fountain pen ink F1, and sulfur in ink F2, enabled effective differentiation. Notably, palladium levels were significantly higher in overlap regions, indicating additive contributions from both inks. These findings emphasize SEM-EDX as a powerful, partially destructive technique for identifying individual ink formulations, distinguishing overlapping inks, and analyzing their interactions, despite its limitation in deciphering diverse texts.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 5","pages":"887 - 893"},"PeriodicalIF":1.1,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145143723","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":"Analytical Control of Functional Materials Based on Rare-Earth Metals Using Mass Spectrometry Methods","authors":"N. A. Korotkova,&nbsp;K. V. Petrova,&nbsp;V. B. Baranovskaya,&nbsp;M. S. Doronina","doi":"10.1134/S1061934825700200","DOIUrl":"10.1134/S1061934825700200","url":null,"abstract":"<p>Rare-earth metals and compounds on their basis are in demand for the development and production of functional materials, such as optical ceramics, permanent magnets, phosphors, catalysts, glasses, alloys, etc. Unique physical and chemical properties of these materials largely depend on their elemental composition (panoramic and target), which must be controlled at all stages of production, from the initial compounds to intermediate and final products. Mass spectrometry with various ionization sources (inductively coupled plasma, vacuum spark discharge, glow discharge, laser source, secondary ion source) and sample introduction systems (solutions’ spraying, laser sampling, electrothermal evaporation) is one of the most promising and in-demand methods for determining target elements with high sensitivity in materials of complex composition. There are a number of other advantages offered by this method, namely the selectivity of the signal from the elements being determined, a possibility of conducting multi-element analyses, and the accuracy of the analysis results. However, materials of complex composition, including those containing rare-earth metals as main elements, require studying the influence of analysis conditions and other factors in order to obtain reliable results and to develop analytical procedures. The article provides a review of publications containing methodological solutions and approaches to overcome the limitations of mass spectrometry with various ionization sources in relation to the analysis of rare-earth metals and functional materials based on them. The review includes Russian and foreign publications from 2014 to 2023.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 5","pages":"785 - 793"},"PeriodicalIF":1.1,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145143828","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":"Arsenic Species Determination in Seaweeds by Ion Chromatography–Inductively Coupled Plasma Mass Spectrometry","authors":"Nguyen Quoc Thang,&nbsp;Hong Khanh Trung,&nbsp;Le Van Tan,&nbsp;Nguyen Thi Kim Phuong,&nbsp;Nguyen Thi Kim Ngan,&nbsp;Tran Quang Hieu","doi":"10.1134/S106193482570025X","DOIUrl":"10.1134/S106193482570025X","url":null,"abstract":"<p>In this research, the most common arsenic species in seaweeds from Ho Chi Minh City (Vietnam) were determined using ion chromatography-tandem inductively coupled plasma mass spectrometry. An optimized extraction procedure was established, involving a 20 mL MeOH : H₂O (1 : 1, v/v) solution at 50°C for 10 min<i>.</i> Chromatographic separation of all the species was achieved in less than 7 min in gradient elution mode using an anion exchange column AS7, and the mobile phase consisted of 300 mM (NH₄)₂CO₃ and 3% MeOH at pH 10.3. The linear range for each arsenic species was from 0.1 to 100 µg/L. The method detection limits for arsenobetaine, dimethylarsinic acid, As(III), monomethylarsonic acid, and As(V) were 21.19, 4.76, 4.29, 2.78, and 2.28 µg/kg, respectively, and the method quantification limits were 100, 15.86, 14.31, and 9.27, 7.62 µg/kg, respectively. The method was validated for accuracy, precision, and specificity. Analysis of 15 seaweed samples revealed the presence of As(III) in some samples, while As(V) was not detected. This study presents a novel method for arsenic determination and provides valuable insights into arsenic levels in seaweed. The developed method offers a valuable tool for assessing arsenic contamination in marine ecosystems and understanding its potential risks to human health.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 5","pages":"877 - 886"},"PeriodicalIF":1.1,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145143857","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":"Erratum to: Ultrasound-Assisted Extraction Combined with Dispersive Liquid-Liquid Microextraction Using Low-Density Solvent—a Novel Approach to Determine Fenvalerate in Strawberry Samples","authors":"Mohammad Rezaee,&nbsp;Davood Ghoddocy Nejad","doi":"10.1134/S106193482504001X","DOIUrl":"10.1134/S106193482504001X","url":null,"abstract":"","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 4","pages":"784 - 784"},"PeriodicalIF":1.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949462","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":"Effect of Organic Matter Content in Water and Sediments on the Recovery of Estrogenic Compounds Extracted by Solid-Phase Extraction and Ultrasound-Assisted Extraction","authors":"José Gustavo Ronderos-Lara,&nbsp;Hugo Saldarriaga-Noreña,&nbsp;Mario Alfonso Murillo-Tovar,&nbsp;Violeta Mugica-Álvarez,&nbsp;Iris J. Montoya-Balbás,&nbsp;Verónica Gisela López-Martínez,&nbsp;Khirbet López-Velázquez,&nbsp;Ernesto Sola-Pérez","doi":"10.1134/S1061934825700066","DOIUrl":"10.1134/S1061934825700066","url":null,"abstract":"<p>This work evaluates the effect of organic matter on the recovery of ibuprofen (<b>IBU</b>), naproxen (<b>NPX</b>), 4-<i>n</i>-nonylphenol (<b>4NP</b>), bisphenol A (<b>BPA</b>), 17β-estradiol (<b>E2</b>) and 17α-ethinylestradiol (<b>EE2</b>) in water and sediment samples. The best solid-phase extraction results were obtained with sample extractions at pH 7, and elution was performed using acetone–MeOH (3 : 2). Recoveries varied between 54.24 ± 0.86% (4NP) and 89.77 ± 5.40% (EE2). Repeatability and reproducibility were below 8.1 and 111.13% (EE2), respectively. The best ultrasound-assisted extraction results were obtained using acetone–MeOH (3 : 2) as the extraction solvent. Recoveries oscillated between 48.8 ± 8.4% (EE2) and 112.6 ± 4.3% (NPX). Repeatability and reproducibility were below 17.21 and 17.84% (BPA), respectively. The validated methods were applied to determine the effect of organic matter on recoveries in surface water and sediment samples impacted by different sources. As a result, in water samples with high organic matter content, recoveries for IBU, NPX, and EE2 increased up to 18, 11, and 22%, respectively. In sediment samples, the recovery of E2 increased up to 43%. Thus, due to the presence of organic matter in samples, it is recommended to explore organic matter content in samples before analysis to minimize errors in determined concentrations.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 4","pages":"634 - 646"},"PeriodicalIF":1.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949439","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":"Separation and Preconcentration of Biologically Active Compounds by Capillary Electrophoresis Using Imidazolium-Based Modifiers","authors":"A. Sh. Ganieva,&nbsp;L. A. Kartsova","doi":"10.1134/S1061934825700170","DOIUrl":"10.1134/S1061934825700170","url":null,"abstract":"<p>A cationic covalent coating based on an imidazolium cation is synthesized for the inner walls of a fused silica capillary. The electroosmotic flow reproducibility, determined using dimethylformamide as a marker, was as high as 99%. The separation conditions for model systems of phenyl- and indolecarboxylic acids—phenylactic, phenylsuccinic, phenylbutanoic, indolelactic, indolepropionic, indoleacrylic, hydroxyindalmic, homogentisic, homovanillic, and hydroxyindoleacetic acids—were optimized for capillary electrophoresis. The optimal background electrolyte consisted of a 10 mM phosphate buffer solution of pH 4.2 with a 10 vol % acetonitrile additive. The resolution factors for adjacent analyte pairs ranged from 1.7 to 18.9. The synthesized coating enabled the in-capillary preconcentration of phenyl- and indolecarboxylic acids. Electrostacking increased analyte concentration factors to 106 to 512 and brought the limits of detection to 4 to 72 ng/mL.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 4","pages":"748 - 755"},"PeriodicalIF":1.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949645","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":"Separation of Oxidative Degradation Products of the Anti-Cancer Drug Gilteritinib Fumarate by Liquid Chromatography with Photodiode Array and Mass Spectrometric Detection","authors":"Pushpa Pilli,&nbsp;Sowmya Chaganti,&nbsp;Vijaya Madhyanapu Golla,&nbsp;Hema Sree Kommalapati,&nbsp;Bhukya Vijay Nayak,&nbsp;Gananadhamu Samanthula","doi":"10.1134/S106193482570011X","DOIUrl":"10.1134/S106193482570011X","url":null,"abstract":"<p>Gilteritinib (<b>GTB</b>) is used for the treatment of refractory or relapsed acute myeloid leukemia and inhibits several receptor tyrosine kinases, including FMS-like tyrosine kinase 3 and AXL. The main objective of the current study was to determine how GTB degrades under forced conditions (hydrolysis, oxidation, and photolysis) in accordance with ICH Q1A and Q1B criteria. Zeneth software was used to predict the in-silico deterioration profile of GTB before the study was carried out. GTB was found to be stable under hydrolytic (acidic, basic, and neutral) and photolytic degradation conditions, but it was labile under oxidative (H₂O₂) conditions, producing three novel degradation products. The degradation products were identified and separated using a Phenomenex Gemini C18 column (250 × 4.6 mm, 5 µm) in a reversed-phase high-performance liquid chromatography with a gradient program. Mobile phases consisted of 10 mM ammonium formate with 0.01% acetic acid (pH unadjusted, %A) and methanol (%B). High-resolution mass spectrometry was used for the structural elucidation of the degradation products. The resulting data enabled the proposal of a mechanism for the formation of the degradation products. Using in silico techniques (DEREK Nexus, SARAH Nexus, and ProTox-3.0), the toxicity and mutagenicity of GTB and its degradation products were predicted. In summary, this study highlights safety monitoring and storage conditions for GTB.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 4","pages":"684 - 692"},"PeriodicalIF":1.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949484","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":"Development and Validation of an Immunochromatography Test System for Determining Okadaic Acid in Seafood","authors":"E. K. Singov,&nbsp;O. S. Morenkov,&nbsp;S. V. Sipin,&nbsp;V. V. Vrublevskaya","doi":"10.1134/S1061934825700169","DOIUrl":"10.1134/S1061934825700169","url":null,"abstract":"<p>Okadaic acid (OA) and its derivatives—dinophysistoxins—belong to the group of diarrhetic shellfish poison toxins (DSP toxins), which are produced by toxin-forming dinoflagellates. When mollusks ingest these algae, DSP toxins accumulate in their adipose tissue and can cause acute poisoning in humans upon consumption. We developed a simple, a sensitive, and a specific test system for the detection and semiquantitatively determination of okadaic acid and its derivatives in mollusks. This system is based on a direct competitive immunochromatographic analysis. The test strips contain three immunoreagent binding lines: a test line, a control line, and an internal reference line. The color intensity of the internal reference line remains independent of the OA concentration in the solution and is comparable to the color intensity of the test line. If DSP toxins are present in a sample, the color intensity of the test line decreases relative to the reference line, enabling toxin detection. Sample preparation involves the extraction of mollusk tissue homogenates with methanol, followed by the dilution of the extract with an analysis buffer. The test strips are manufactured in a dipstick format, and the analysis procedure consists of immersing part of the strip into a sample for a few seconds, with results processed after 30 min. The total analysis time, including sample preparation, is approximately 1 h. The test system reliably detects and semiquantitatively determines okadaic acid in various mollusks, including oysters, mussels, venus clams, whelks, and sea scallops, at toxin concentrations of up to 40 ng/g using visual result detection and up to 10 ng/g using instrumental registration. These limits of detection are significantly lower than the maximum permissible concentration for okadaic acid set by the World Health Organization and Rospotrebnadzor (160 ng/g). In addition to okadaic acid, the test system can also detect its derivatives, dinophysistoxin-1 and dinophysistoxin-2, in mollusks. The developed immunochromatographic test system can be used for monitoring OA-group toxin levels in mollusks in Russia.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 4","pages":"738 - 747"},"PeriodicalIF":1.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949579","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":"Main Strategies of the Sample Preparation of Biological Samples Containing Nanoparticles for Their Subsequent Analysis by Single Particle Inductively Coupled Plasma Mass Spectrometry: A Mini-Review","authors":"O. N. Grebneva-Balyuk,&nbsp;M. S. Kiseleva,&nbsp;I. V. Kubrakova","doi":"10.1134/S1061934825700042","DOIUrl":"10.1134/S1061934825700042","url":null,"abstract":"<p>The characterization of highly dispersed materials and nanoparticles (NPs), as well as the investigation of their transformations in biological systems, constitute a critical aspect of research aimed at assessing the potential for active NP applications in biomedicine and pharmacology. A promising method for characterizing NPs involves single particle inductively coupled plasma mass spectrometry (SP ICP MS). This technique enables the determination of nanoparticle masses at the femtogram level and gives information on their distribution by the analyte form (soluble ionic or nanoscale), size, and quantity within the analyzed sample. Sample preparation for an SP ICP MS analysis is based on the quantitative extraction of NPs from a biological sample while preserving their characteristics. Liquid samples for analysis are prepared by dilutions, involving filtration, centrifugation, sedimentation, and various fractionation and separation techniques. Enzymatic and alkaline hydrolysis have been applied to the decomposition of biological tissues. The discussion addresses the capabilities and limitations of primary sample preparation methods, using biomaterials containing gold and silver NPs as examples. Particular attention is given to techniques that do not alter the analyte, such as dilution and filtration. A possibility of analyzing iron oxide-based materials, relevant to biomedical research, using SP ICP MS is noted, along with the challenges associated with such analyses. The combination of laser ablation (as a sampling method) with SP ICP MS is shown to be a promising approach to studying the spatial distribution of NPs in biological systems.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 4","pages":"608 - 622"},"PeriodicalIF":1.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949584","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":"Identification and Detection of Adulterations of Salmon Caviar by PCR, IR Spectrometry, and Digital Coloriometry","authors":"V. G. Amelin,&nbsp;O. E. Emel’yanov,&nbsp;A. V. Tret’yakov,&nbsp;M. A. Gergel’,&nbsp;E. V. Zaitseva","doi":"10.1134/S1061934825700194","DOIUrl":"10.1134/S1061934825700194","url":null,"abstract":"<p>A possibility of identifying and establishing adulterations of salmon caviar by a simple and an available method using PCR, Fourier transform IR spectrometry, digital colorimetry with the chemometric processing of the analysis results is shown. The PCR method is used to determine the species of salmon caviar. No salmon DNA in the studied caviar samples, as well as the presence of DNA of other fish, indicates the adulteration of the caviar products. Near- and mid-region Fourier transform infrared spectroscopy makes it possible to distinguish between the natural and imitation caviar after processing diffuse reflectance spectra by principal component analysis and hierarchical cluster analysis. The above methods are combined with a simpler and a cheaper colorimetric analysis method. Hand-made devices with LEDs emitting in the UV and IR regions are used. The analytical signal is recorded using smartphones with specialized applications. Chemometric processing of the spectral characteristics of the samples makes it possible to distinguish natural caviar from imitation and structured caviar: in the principal component analysis and hierarchical cluster analysis, points of the analyzed samples are located in different quadrants and clusters.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 4","pages":"772 - 783"},"PeriodicalIF":1.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949451","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}