Journal of Analytical Chemistry最新文献

{"title":"Determination of the Oxidative Damage Markers of Nucleic Acids 8-Hydroxyguanosine and 8-Hydroxy-2'-Deoxyguanosine in Urine Using High-Performance Liquid Chromatography with Tandem Mass-Spectrometric Detection","authors":"E. I. Savelieva,&nbsp;G. V. Karakashev,&nbsp;M. V. Belyakov,&nbsp;A. S. Venediktov,&nbsp;A. N. Bikbulatov","doi":"10.1134/S1061934825700674","DOIUrl":"10.1134/S1061934825700674","url":null,"abstract":"<p>Products of oxidative damage to nucleic acids are considered as relatively stable biomarkers in the diagnosis of negative consequences of oxidative stress. The concentrations of biomarkers of oxidative degradation of DNA (8-hydroxy-2'-deoxyguanosine, 8-OHdG) and RNA (8-hydroxyguanosine, 8-OHG) in biofluids increased when the body was exposed to toxic compounds, radiation, and other negative factors associated with oxidative stress. Urine is considered as a priority matrix for biomonitoring the consequences of oxidative stress because of noninvasive sampling and higher concentrations of the target analytes. We developed a procedure for the combined determination of 8-OHdG and 8-OHG in urine using HPLC–MS/MS analysis. A structurally similar exogenous compound, 8-[(1-hydroxybutan-2-yl)amino]-1,3,7-trimethyl-1-purine-2,6(3<i>H</i>,7<i>H</i>)-dione, was selected as an internal standard. The measurement range from 1 to 50 ng/mL was set for both analytes. A solid-phase extraction procedure on a hydrophilic–lipophilic balance (HLB) sorbent in the analyte retention mode was optimized to prepare biological samples for analysis. With the use of high-resolution HPLC–MS/MS technique, the error of analysis did not exceed 25% over the entire analytical range. A total of 130 urine samples of chemical plant workers aged 20 to 70 years without diagnosed systemic diseases were analyzed. The 8-OHdG and 8-OHG contents of the urine samples ranged from 1 to 20 and from 2 to 12 ng/mL, respectively. The dependence of the concentrations of both biomarkers in urine on the age of the workers was established.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 8","pages":"1402 - 1410"},"PeriodicalIF":1.1,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144868735","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":"Preconcentration of Quinolones on Magnetic Hypercrosslinked Polystyrene before Their Determination by High-Performance Liquid Chromatography in Milk","authors":"Ya. A. Kulinich,&nbsp;I. D. Puryskin,&nbsp;V. V. Tolmacheva,&nbsp;A. O. Melekhin,&nbsp;V. V. Apyari,&nbsp;S. G. Dmitrienko","doi":"10.1134/S1061934825700649","DOIUrl":"10.1134/S1061934825700649","url":null,"abstract":"<p>Magnetic hypercrosslinked polystyrene (<b>MHCPS</b>) is proposed for the group adsorption and preconcentration of quinolones. The conditions for magnetic solid-phase extraction are selected as follows: 25 mL of solution (pH 6), sorbent mass 20 mg, and sorption time 20 min. The analytes have been desorbed with 2 mL of methanol. It is shown that the sorbent provides the quantitative extraction of all 23 studied compounds not only from aqueous solutions, but also from milk, bypassing the deproteinization stage. The determination is carried out by HPLC-tandem mass spectrometry using matrix calibration. The limits of detection and determination for quinolones are 0.012–0.12 and 0.04–0.4 μg/L, respectively, which are below their maximum residue levels in milk.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 8","pages":"1368 - 1376"},"PeriodicalIF":1.1,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144868738","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":"Ionic Liquids as Promising Functional Materials for the Microextraction of Steroid Hormones","authors":"A. T. Araslanova,&nbsp;M. Vasilenko,&nbsp;E. A. Bessonova,&nbsp;L. A. Kartsova","doi":"10.1134/S1061934825700601","DOIUrl":"10.1134/S1061934825700601","url":null,"abstract":"<p>Prospects for the use of imidazolium ionic liquids (<b>ILs</b>) as extractants of sex steroid hormones (estrogens and androgens) in microextraction methods (dispersive liquid–liquid microextraction, <b>DLLME</b>, and magnetic solid-phase microextraction, <b>mSPME</b>) are identified. The key parameters of DLLME using C₆MImNTf₂ ionic liquid that affect extraction efficiency are optimized using the design of experiments technology. High recoveries (88–99%) are achieved. An approach of dynamic IL immobilization on the surface of magnetic nanoparticles (<b>MNPs</b>) for the extraction of steroids under mSPME conditions is proposed. Two types of MNP pre-coating are studied: hydrophilic based on silica and hydrophobic with oleic acid. The capabilities of C₈MImBF₄ ionic liquid as a MNP surface modifier for the efficient extraction of steroids are revealed. Optimum conditions provided high degrees of recovery (83–97%), with an exception of estriol (60%). The limits of detection are 0.26–1.29 ng/mL. Limitations of the method related to the partial removal of IL from the surface of NPs are revealed; they reduce the reproducibility of the results for estriol.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 8","pages":"1331 - 1344"},"PeriodicalIF":1.1,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144868892","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":"Features of Preconcentration and Determination of PAHs in Soils with High Organic Matter Content by Gas Chromatography–Mass Spectrometry","authors":"Z. A. Temerdashev,&nbsp;S. K. Ovsepyan,&nbsp;T. N. Musorina,&nbsp;I. G. Korpakova","doi":"10.1134/S1061934825700662","DOIUrl":"10.1134/S1061934825700662","url":null,"abstract":"<p>Specific features of the preconcentration and determination of polycyclic aromatic hydrocarbons (PAHs) in humus-rich soils by gas chromatography–mass spectrometry (GC–MS) are studied. The QuEChERS technique and dispersive liquid–liquid microextraction (DLLME) were employed to extract PAHs from soils using acetone and binary extractants of various compositions, including acetonitrile–dichloromethane, acetonitrile–acetone, acetone–hexane, acetone–chloroform, acetone–dichloromethane, and ethyl acetate–dichloromethane. Recoveries of low- and medium-molecular-weight PAHs using these solvent mixtures reached approximately 100%, while the acetone–dichloromethane mixture yielded over 90% recovery for high-molecular-weight PAHs. Under optimized GC–MS conditions with QuEChERS extraction, the limits of quantification (LOQ) for fluoranthene, pyrene, chrysene, and triphenylene reached 5 µg/kg, and for the remaining PAHs, 10 µg/kg in humus-rich soils. It was shown that the reliable GC–MS determination of lower concentrations of PAHs requires both the elimination of the matrix effect and the preconcentration of the analytes. The sequential application of QuEChERS and DLLME techniques enabled a decrease in the limits of quantification by GC–MS to 1.8 µg/kg for fluoranthene, pyrene, chrysene, and triphenylene, and to 3.5 µg/kg for the remaining PAHs. The optimized procedure for PAH determination in humus-rich soils was validated using real chernozem samples.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 8","pages":"1389 - 1401"},"PeriodicalIF":1.1,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144869113","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":"Multielemental Analysis of Tellurium Dioxide with Sample Matrix Preseparation by Reactive Distillation","authors":"A. R. Tsygankova,&nbsp;T. Ya. Guselnikova,&nbsp;V. A. Oshustanova","doi":"10.1134/S1061934825700637","DOIUrl":"10.1134/S1061934825700637","url":null,"abstract":"<p>A method is proposed for matrix separation from a sample of tellurium dioxide TeO₂ as tellurium tetrachloride based on reactive distillation in a flow reactor at 240°C using gaseous chlorine as a chlorination agent. The behavior of 59 impurities is studied, and it was found that As, Au, B, Bi, Cu, Ga, In, Mo, Nb, Pb, Re, Ru, Sb, Se, Sn, Ta, Ti, V, W, and Zn were lost completely or partially, whereas Ag, Al, Ba, Be, Ca, Cd, Ce, Co, Cr, Dy, Er, Eu, Gd, Ir, Hf, Ho, K, La, Li, Lu, Mg, Mn, Na, Nd, Ni, P, Pd, Pr, Pt, Rb, Rh, Sc, Sm, Sr, Tb, Tm, Y, Yb, and Zr were retained in the concentrate by more than 75%. The impurity content of the concentrate was determined by inductively coupled plasma atomic emission spectrometry. Accuracy was confirmed by the spike experiment and by comparison with the results of analyses without preconcentration. The limits of detection are in the range from 2 × 10^–8 to 8 × 10^–6 wt %, intralaboratory precision is better than 31%.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 8","pages":"1360 - 1367"},"PeriodicalIF":1.1,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144868739","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 Ethanol in Soft Drinks by Gas Chromatography Using Headspace Single-Drop Microextraction","authors":"O. V. Rodinkov,&nbsp;K. N. Davletbaeva","doi":"10.1134/S1061934825700625","DOIUrl":"10.1134/S1061934825700625","url":null,"abstract":"<p>A simple and a rapid procedure for the gas-chromatographic determination of ethanol in soft drinks is proposed (kvass, grape juice, non-alcoholic beer) based on the headspace microextraction of an analyte into a drop (1 μL) of distilled water located above the surface of the analyzed liquid on the tip of a needle of a standard microsyringe for gas chromatography. The limit of detection for ethanol is (3–6) × 10^–5 vol %, the time of a replicate determination, including headspace extraction, does not exceed 5 min. 2-Propanol, not detected in the beverages, is used as an internal standard. The accuracy of the procedure is confirmed by the added–found method, the relative standard deviation does not exceed 7% at the ethanol concentration in the sample 10^–2 vol %.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 8","pages":"1354 - 1359"},"PeriodicalIF":1.1,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144868740","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":"Efficient and Selective Colorimetric Sensing of Bisulfate, Ferrous, and Cupric Ions by a Pyrazole-Derived Schiff Base","authors":"Hafiz Muhammad Junaid,&nbsp;Muhammad Hamza Mukhtar,&nbsp;Madeeha Batool","doi":"10.1134/S1061934825600726","DOIUrl":"10.1134/S1061934825600726","url":null,"abstract":"<p>Pyrazole-derived Schiff bases are mostly designed for the optical sensing of ionic species. In this research, a pyrazole-based Schiff base, 4-(4-methoxybenzylideneamino)-1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H)-one (<b>MBz-AAP</b>), has been studied for its optical sensing properties towards various ionic species, including heavy metal ions and anions. Among these species, this probe exhibits a color change from colorless to maroonish-red for Fe²⁺ and Cu²⁺ ions, and colorless to yellow for <span>({text{HSO}}_{4}^{ - })</span> ions. These optical changes are found to be consistent with red shifts in the ultraviolet-visible absorption spectrum of MBz-AAP from 334 to 504, 510, and 387 nm for Fe²⁺, Cu²⁺, and HSO₄^– ions, respectively. Limits of detection (<b>LOD</b>) of MBz-AAP for Fe²⁺, Cu²⁺, and <span>({text{HSO}}_{4}^{ - })</span> ions are calculated to be 2.45, 3.34, and 2.24 μM, respectively. These LODs for Fe²⁺ and Cu²⁺ are much lower than their allowable limits in drinking water, i.e., 5.36 and 31.5 μM, respectively. Moreover, the stoichiometric binding ratios of Fe²⁺, Cu²⁺, and <span>({text{HSO}}_{4}^{ - })</span> with MBz-AAP are determined to be 1 : 1, with binding constants of 5.0 × 10³, 1.6 × 10³, and 7.05 × 10³ M^–1, respectively.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 8","pages":"1422 - 1433"},"PeriodicalIF":1.1,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144868792","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":"Regularities of Retention of Alcohols, Ketones, and Sugars on a Sulfonic Acid Cation Exchanger in H+-, Ca2+- and La3+-Forms","authors":"A. Yu. Laptev,&nbsp;S. S. Balashova,&nbsp;N. B. Rozhmanova,&nbsp;A. V. Sevko,&nbsp;V. D. Kazakova,&nbsp;P. N. Nesterenko","doi":"10.1134/S1061934825700650","DOIUrl":"10.1134/S1061934825700650","url":null,"abstract":"<p>The chromatographic retention of alcohols, ketones, alditols, and carbohydrates on a cation exchanging column (200 × 4.6 mm, Sevko AA) packed with sulfonated poly(styrene-divinylbenzene) with a crosslinking degree of 10% and a particle diameter of 7 μm saturated with various counterions (H⁺, Ca²⁺ and La³⁺) is studied in the ligand exchange chromatography version. The sorbent in the Ca²⁺ form shows higher retention times and selectivity in the separation of carbohydrates and ethylene glycols. The sorbent in the La³⁺ form provides a strong retention and a better selectivity for the separation of alditols. A possibility of using this column for determining carbohydrates in food products (juice, honey) using refractometric detection is shown.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 8","pages":"1377 - 1388"},"PeriodicalIF":1.1,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144869112","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":"A Novel Quadriplex Reverse Transcription PCR Assay for Robust SARS-CoV-2 Diagnosis and Variant Detection: Experimental Optimization for Enhanced Sensitivity and Specificity","authors":"Nahla O. Mousa,&nbsp;Marwan Osama,&nbsp;Hala Talkhan,&nbsp;Ahmed Osman","doi":"10.1134/S1061934825700704","DOIUrl":"10.1134/S1061934825700704","url":null,"abstract":"<p>Severe acute respiratory syndrome coronavirus 2 (<b>SARS-CoV-2</b>) is a novel coronavirus that has been identified as the causative agent of an ongoing global pandemic of acute respiratory distress syndrome, coronavirus disease 2019. Ranked as one of the top priorities is developing an accurate, reliable, and affordable laboratory diagnostic test for pathogen detection to facilitate disease tracking. In this study, a multiplex-based assay to detect SARS-CoV-2 using four primers/probes to amplify regions of the spike (S), nucleocapsid (N), and envelope (E) protein-coding genes, along with amplifying region of the 3' untranslated region (<b>UTR</b>) was designed and developed. To provide accurate detection of different SARS-CoV-2 variants, an in silico design and validation pipeline was utilized. These included multi-sequence alignments with Clustal Omega, specificity verification by the Basic Local Alignment Search Tool (primer-BLAST), and computational performance verification using Biopython. The primers and hydrolysis probes designed were experimentally tested against more than two million SARS-CoV-2 genome sequences obtained from the National Center for Biotechnology Information Virus Database, with &gt;97% specificity across 2200 lineages, including all of the significant variants of concern and variants of interest. The experimental validation phase included synthetic SARS-CoV-2 constructs and ribonucleic acid samples from nasopharyngeal swabs of 20 patients, including both symptomatic and asymptomatic cases. The assay displayed 100% sensitivity and specificity, with the limit of detection as low as 10 copies/mL, which surpassed the detection limits of some commercially available reverse transcription quantitative polymerase chain reaction (RT-qPCR) kits. Amplification efficiency was optimized for all targets, ranging from 94.92% for the N gene, 98.84% for the S gene, 81.75% for the E gene, to 82.14% for the 3′UTR genes. Assay selectivity was verified by cross-reactivity against common respiratory viruses—SARS-CoV-1, Middle East respiratory syndrome coronavirus, Influenza A/B, and human coronaviruses (HCoV-229E, HCoV-NL63, HCoV-OC43, and HCoV-HKU1)—and no off-target signal was observed. The ability to detect multiple genomic regions renders the assay resilient to mutation-based primer mismatch, making it extremely suitable for clinical diagnostics, epidemiological surveillance, and variant monitoring.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 8","pages":"1471 - 1482"},"PeriodicalIF":1.1,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144869124","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":"Modeling and Simulation of an Electroosmotically Driven Micromixer with Two Rectangular Obstacles Inside the Channel","authors":"Elnaz Poorreza","doi":"10.1134/S1061934825700716","DOIUrl":"10.1134/S1061934825700716","url":null,"abstract":"<p>Micromixers are widely employed within the domains of biochemistry, drug delivery, and biomedical applications, among others. The phenomenon of induced-charge electroosmosis has garnered significant attention from the microfluidic research community over the past decade. The model put forth leverages the principles of electroosmosis to enhance the process of fluid mixing. This system incorporates a time-varying electric field, wherein the resulting electroosmosis disturbs the parallel streamlines that are characteristic of the otherwise highly organized laminar flow regime. A sinusoidal electric potential of 0.1 V and a frequency of 9 Hz are applied across the electrodes. In order to further augment the mixing efficiency, two congruent obstacles are judiciously positioned within the channel. The findings indicate that the micromixer exhibits an impressive mixing efficiency approaching 95% and possesses potential applications across diverse fields, including biochemistry and the biomedical sciences.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 8","pages":"1483 - 1491"},"PeriodicalIF":1.1,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144869114","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}