Journal of Analytical Chemistry最新文献

{"title":"Simultaneous Determination of Nickel(II), Copper(II), and Cobalt(II) in Environmental Samples at Trace Levels by Reversed-Phase High-Performance Liquid Chromatography Using Shiff Base Complexes","authors":"M. Umut Konanç,&nbsp;Adem Asan","doi":"10.1134/S1061934825700303","DOIUrl":"10.1134/S1061934825700303","url":null,"abstract":"<p>A new method for the simultaneous determination of Ni(II), Cu(II), and Co(II) ions in environmental samples by reversed-phase liquid chromatography was developed. The developed method is based on the synthesis of the quadrivalent Schiff base 6,6'-((1E,1'E)-(ethane-1,2-diylbis(azaneylylidene))bis(methaneylylidene))bis(3-methoxyphenol) by the condensation reaction between 2-hydroxy-4-methoxybenzaldehyde and ethylenediamine. The resulting Schiff base was used as a chelating agent to convert the targeted ions into metal-ligand complexes within 1 min, which were extracted on an octadecylsilane (<b>ODS</b>) solid-phase extraction mini-column and then injected into a reversed-phase high-performance liquid chromatography system. Sufficient separation of the metal-ligand complexes was achieved on a GL Sciences Intersil ODS-3 column with a mobile phase composition of methanol-acetonitrile-water (30 : 30 : 40, v/v) within 6 min and detection by an ultraviolet detector at 254 nm. The limits of detection were found to be 0.45, 0.40, and 1.47 µg/L for Co²⁺, Cu²⁺, and Ni²⁺, respectively. Recoveries from water samples ranged from 97.4 to 103.6%, with relative standard deviation values between 0.4 and 1.7%. While the targeted metal ions were not detected in a sample from the remote upstream area of the Kabaca Stream (Artvin, Turkey), concentrations were found to be 116.4 µg/L for Cu²⁺ and 32.9 µg/L for Ni²⁺ in a sample taken from the Kabaca Stream near the industrial area (Artvin, Turkey). Co²⁺ was below the limit of detection in both cases. In addition, the developed method was also validated using the inductively coupled plasma optical emission spectrometry technique.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 5","pages":"894 - 902"},"PeriodicalIF":1.1,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145143829","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":"Simulation and Optimization of a Low-Voltage Microseparator Based on Dielectrophoresis Forces for Blood Cell Separation","authors":"Elnaz Poorreza,&nbsp;Noushin Dadashzadeh Gargari","doi":"10.1134/S1061934824605280","DOIUrl":"10.1134/S1061934824605280","url":null,"abstract":"<p>The objective of this investigation is to develop optimization approaches for the separation of platelets from red blood cells (<b>RBC</b>s). A novel microfluidic device with triangular electrodes operating at a low voltage of 1.5 V and a frequency of 100 kHz is proposed for the separation of platelets and RBCs using dielectrophoresis (<b>DEP</b>) force. Using of a low voltage ensures the preservation of the viability of biological cells, which is a crucial factor for medical applications. Through a comparative investigation utilizing the finite element method, the impact of varying electrode dimensions on the effective separation of particles is demonstrated. Profiles of electric field, pressure, and DEP force acting on two particles are presented through simulation.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 5","pages":"801 - 812"},"PeriodicalIF":1.1,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145143855","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 Sensitive Headspace Gas Chromatography Method for the Determination and Quantitation of Acryloyl Chloride","authors":"Nicolette Fernandes,&nbsp;Lin Lin,&nbsp;Lin Chen,&nbsp;Yanlou Wang,&nbsp;Ti Zhang,&nbsp;Wang Zheng,&nbsp;Rong Yu,&nbsp;Maria Gerasi,&nbsp;Steven Mathieu,&nbsp;Erin O’Brien","doi":"10.1134/S106193482460433X","DOIUrl":"10.1134/S106193482460433X","url":null,"abstract":"<p>This paper describes a simple, sensitive, and specific headspace gas chromatography method that has been developed and validated for the quantitation of acryloyl chloride, a potential mutagenic impurity in a drug substance. Using ethanol as the derivatizing agent, acryloyl chloride is converted to ethyl acrylate, which is quantitated with headspace gas chromatography. Quantitation was performed with an external standard by thermostating the sample and standard before analysis, allowing for high extraction of the analyte in the gas phase of the headspace vial. The method is sensitive, with a limit of quantitation (<b>LOQ</b>) of 10 ppm for acryloyl chloride in the drug substance. This method, combined with its high sensitivity and the incorporation of headspace sampling, represents the first of its kind for quantifying acryloyl chloride at low levels in a pharmaceutical matrix. The performance of the method was evaluated by assessing parameters like specificity, linearity, precision, LOQ, and solution stability. The developed method was successfully used to quantify acryloyl chloride accurately in samples of the drug substance. The specificity, sensitivity, and simplicity of this method make it suitable for the quantitation of acryloyl in the drug substance at trace levels. This method is applicable to other drug substance matrices with minimal method adjustments.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 5","pages":"920 - 930"},"PeriodicalIF":1.1,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145143721","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 of a Data Processing Algorithm for the Electronic Nose Based on Piezoelectric Sensors in Blood Sample Analysis without Sample Preparation: A Pilot Study","authors":"T. A. Kuchmenko,&nbsp;D. A. Menzhulina","doi":"10.1134/S1061934825700285","DOIUrl":"10.1134/S1061934825700285","url":null,"abstract":"<p>The study presents the first results of blood analysis conducted without sample preparation using a portable “electronic nose” based on piezoelectric sensors in hospital departments of various specialization. Over 6 months, clinical laboratory personnel at a regional hospital performed parallel blood analyses using both traditional and sensor-based methods. The study evaluates the impact of environmental conditions—including room temperature, measurement repetition frequency, and the nature of piezoelectric sensor electrode modifiers—on the signal reproducibility within the sensor array. The authors propose effective approaches and algorithms for the processing of the data of a multidimensional piezoelectric sensor array in the detection of the volatile organic compound (VOC) profile of small-volume blood samples (≤0.5 mL). For blood analysis without sample preparation, second-grade distilled water serves as an effective internal standard under laboratory conditions. The study includes blood samples from 250 patients, with the sensor array reliably differentiating cases of pronounced inflammatory pathologies, oncology, severe renal dysfunction, and extreme stress conditions (e.g., surgical procedures, traffic accidents with fatal injuries, or burns). The proposed parameter also identifies other pathological conditions; however, its magnitude varies based on individual patient characteristics, comorbidities, disease compensation, and the severity of pathological processes on admission (e.g., type 2 diabetes mellitus). A component-by-component analysis of VOC profiles for samples with significant pathologies will be addressed in a subsequent report. The study optimizes VOC detection methods, including measurement mode and repetition frequency, and introduces simple yet effective algorithms for the processing of sensor array data.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 5","pages":"942 - 957"},"PeriodicalIF":1.1,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145143722","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":"Spectrophotometric Determination of Lead in Wastewater from the Battery Industry Based on the Interaction with EDTA Disodium Salt","authors":"Afaf Lalmi,&nbsp;Chahrazad Amrane,&nbsp;Sabrina Tamersit,&nbsp;Salima Hamadouche,&nbsp;Ammar Ouahab","doi":"10.1134/S1061934824603943","DOIUrl":"10.1134/S1061934824603943","url":null,"abstract":"<p>In addressing the imperative need to assess lead (Pb) concentrations in water due to its heightened toxicity even at minimal levels, this study seeks to overcome challenges in current testing methodologies. Existing approaches often rely on expensive equipment, limiting their accessibility and widespread application. To address this issue, this investigation introduces a simple, rapid, and selective spectrophotometric method for the precise quantification of Pb²⁺ in aqueous solutions. This method is based on the reaction of Pb²⁺ with ethylenediaminetetraacetic acid (<b>EDTA</b>) in an ammonia buffer solution, with an absorption maximum observed at 240 nm. The study was conducted under varying parameters, including EDTA concentration, pH of the medium, the presence of organic compounds, and interference effects. The calibration curve demonstrated linearity within the range of 0.5–20 mg/L, with a correlation coefficient (<i>R</i>²) of 0.999, using an ultraviolet-visible spectrophotometer at a λ_max of 240 nm. The apparent molar absorption coefficient and limit of detection of Pb²⁺ were found to be 2.19 × 10⁴ L/ (mol cm) and 0.44 mg/L, respectively. The relative standard deviation for five replicates was less than 2%. Crucially, interference from other ions (Na⁺, K⁺, Ca²⁺, Mg²⁺, Cu²⁺, Zn²⁺, Fe²⁺, Co²⁺, Cd²⁺, and Al³⁺) was negligible. The proposed method was successfully applied to determine Pb²⁺ concentrations in battery wastewater samples. The results obtained with the present method were comparable to those from atomic absorption spectroscopy and exhibited high accuracy and excellent precision. These compelling results underscore the method’s efficacy, establishing it as a practical and cost-effective approach for diverse Pb²⁺ determination applications.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 5","pages":"822 - 828"},"PeriodicalIF":1.1,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145143854","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 Triangular Silver Nanoplates for the Detection of Trace Lead Ions","authors":"Ling-ling Zhang,&nbsp;Yun-fei Long,&nbsp;Fu-chun Xie","doi":"10.1134/S1061934824605413","DOIUrl":"10.1134/S1061934824605413","url":null,"abstract":"<p>In an acidic medium (pH 2.56), the silver atoms at the three vertices of triangular silver nanosheets (<b>TAg-NP</b>s) are highly active, making them prone to oxidation by oxygen in the air, which converts them into Ag⁺. This oxidation alters the morphology of TAg-NPs from triangles to disk or spherical shapes, resulting in a blue shift in the maximum absorption wavelength (λ_max) of TAg-NPs. However, in Britton –Robison buffer solution <b>(BR)</b> at pH 2.56, when a small amount of Pb²⁺ is present in the solution, the <span>({text{PO}}_{4}^{{3 - }})</span> ionized from the BR can react with Pb²⁺ to produce Pb₃(PO₄)₂ precipitates, which adhere to the surface and vertices of TAg-NPs, leading to aggregation among them, subsequently inhibiting the corrosion of TAg-NPs in the acidic medium. Moreover, the negatively charged phosphate ions (<span>({text{PO}}_{4}^{{3 - }})</span>) can attract multiple cations simultaneously. For instance, two <span>({text{PO}}_{4}^{{3 - }})</span> ions can react with three Pb²⁺ ions to form a larger complex, causing the TAg-NPs to aggregate. Consequently, both the morphology and the maximum absorption wavelength of TAg-NPs undergo significant changes as the concentration of Pb²⁺ increases in the presence of BR at pH 2.56. Consequently, the color of TAg-NPs shifts gradually, and the change in maximum absorption wavelength (Δλ) between TAg-NPs/Pb²⁺/BR and TAg-NPs/BR solutions correlates with the concentration of Pb²⁺. Based on this, a new method for detecting Pb²⁺ has been established that is simple, rapid, and sensitive.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 5","pages":"839 - 848"},"PeriodicalIF":1.1,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145143856","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":"Retention Behavior of Nitrogen-Containing Heterocyclic Compounds in Reversed-Phase and Hydrophilic HPLC–MS","authors":"O. I. Grinevich,&nbsp;A. Yu. Sholokhova,&nbsp;D. D. Matyushin","doi":"10.1134/S1061934825700261","DOIUrl":"10.1134/S1061934825700261","url":null,"abstract":"<p>Aromatic five- and six-membered nitrogen-containing heterocyclic compounds are biologically active substances widely used in biochemistry and medicine. In addition, such compounds are known as ecotoxicants formed during oxidative processes in industrial wastewaters. High-performance liquid chromatography–mass spectrometry has been widely used to determine nitrogen-containing heterocycles in various complex mixtures; octadecyl silica is used as the main sorbent for chromatographic separation. However, with octadecyl silica, satisfactory separation cannot be achieved in all cases when highly polar isomeric molecules are present, and more selective chromatographic approaches are needed. One such approach is hydrophilic chromatography, which enables the separation of polar compounds. The aim of this work was to characterize and compare the retention of several five- and six-membered nitrogen-containing heterocyclic compounds in reversed-phase and hydrophilic liquid chromatography modes coupled with mass spectrometric detection. Additionally, spectrophotometric measurements were carried out at a wavelength of 210 nm. Octadecyl- and bare silica adsorbents were used to achieve the aim of the work. High-resolution mass spectrometric detection in the electrospray ionization mode was performed. Nineteen nitrogen-containing heterocyclic compounds were studied. Formic acid and diethylamine were chosen as acid–base additives to aqueous acetonitrile mobile phases. Ammonium formate was used as an additive in the hydrophilic chromatography mode. In the reversed-phase chromatography mode, it was shown that the injection of a 0.1% formic acid aqueous solution improved the ionization and signal intensity of the mass spectrometer, but not always allow achieving sufficient isomer separation in elution from the octadecyl silica surface. The injection of a 0.01% diethylamine solution does not result in a pronounced improvement in the separation compared to the mobile phase without modifiers. The use of bare silica in the hydrophilic chromatography mode allows the separation of isomeric five-membered heterocycles by obtaining narrow symmetric peaks but does not lead to the selective separation of isomeric diazines. Thus, the retention of electrospray-ionized nineteen nitrogen-containing heterocyclic compounds in reversed-phase HPLC and HILIC modes was investigated in this work. It was found that hydrophilic chromatography on bare silica allows the satisfactory separation of isomeric five-membered heterocyclic compounds of different classes. For the separation of six-membered heterocycles, satisfactory separation is achieved by elution from the surface of octadecyl silica using an aqueous acetonitrile mobile phase without modifiers.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 5","pages":"903 - 911"},"PeriodicalIF":1.1,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145143858","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 Critical Review of Methods for Hold-Up Time (Volume) Determination","authors":"V. I. Deineka","doi":"10.1134/S1061934825700212","DOIUrl":"10.1134/S1061934825700212","url":null,"abstract":"<p>Known methods for determining hold-up time, essential for calculating retention factors and related chromatographic patterns, are reviewed. The retention factor, initially defined in the theoretical plate model for chromatography on non-porous sorbents, can be adapted to porous sorbents containing mobile phase components in stagnant zones within the sorbent pores. However, in this case, the zone of an unretained solute moves slower than the actual velocity of the mobile phase. The most commonly used approaches from previously proposed methods are considered, taking into account new experimental data. The possible presence of gallery pores in sorbents raises concerns about the gravimetric method. Furthermore, this method, like many others, does not take into account differences in retention mechanisms between adsorption and absorption. The use of solvents wetting the stationary phase likely leads to the penetration of solvent molecule into the attached phase and should yield a hold-up volume applicable to the absorption mechanism. If the solvent poorly wets the stationary phase, the obtained hold-up volume loses clear physical meaning. Calculations of hold-up time based on the retention of deuterated water are more appropriate to the determination of hold-up time in adsorption-based retention but may result in overestimated values due to water adsorption on residual silanol groups. The use of deuterated organic solvents for the same purpose raises additional concerns. Using inorganic salts as hold-up volume markers may lead to inaccuracies due to exclusion effects, which should also be considered in other methods. The homologous series method is not entirely reliable for several reasons discussed in the text. Similarly, the system peak method cannot provide unambiguous confirmation, as it may correspond to retention with an uncertain degree of exclusion effects. Consequently, the problem remains unresolved, and the development of new specialized approaches is required.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 5","pages":"794 - 800"},"PeriodicalIF":1.1,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145144041","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 of Turmeric and Revelation of Adulterations by Digital Colorimetry and Near-IR Spectrometry","authors":"O. E. Emel’yanov,&nbsp;V. G. Amelin,&nbsp;A. V. Tret’yakov","doi":"10.1134/S1061934825700236","DOIUrl":"10.1134/S1061934825700236","url":null,"abstract":"<p>A possibility of identifying turmeric and establishing its adulterations by simple and available methods using IR spectrometry, digital colorimetry, and chemometric spectral data processing is shown. Near-IR spectrometry enabled the differentiation of samples of turmeric powder purchased in India and prepared by grinding roots and commercial samples, and also their distinguishing from samples containing flour, starch, bread crumb, and chalk impurities by analyzing diffuse reflection spectra using principal component analysis, hierarchical cluster analysis, and soft independent modelling of class analogy. The same approaches were applied to a simpler and a less expensive colorimetry method. Chemometric processing of the data obtained confirmed the absence of similarity between the analyzed turmeric samples and samples with additives and made it possible to determine impurities using multivariate regression analysis algorithms. A comparison of the results obtained by IR spectrometry and digital colorimetry demonstrated their equivalent efficiency, so that a more available colorimetry method can be recommended for the routine quality control and the detection of turmeric adulterations.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 5","pages":"829 - 838"},"PeriodicalIF":1.1,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145143718","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":"Experimental and Theoretical Investigations of Singly Charged Metal-Argide Ions ArM+ Manifestation in Inductively Coupled Plasma Mass Spectrometry","authors":"A. A. Pupyshev,&nbsp;P. V. Kel’,&nbsp;M. Yu. Burylin,&nbsp;A. G. Abakumov,&nbsp;P. G. Abakumov,&nbsp;M. A. Maltcev,&nbsp;I. V. Morozov,&nbsp;E. L. Osina","doi":"10.1134/S1061934825700297","DOIUrl":"10.1134/S1061934825700297","url":null,"abstract":"<p>Singly charged metal-argide ions ArM⁺ (M—a metal atom) create significant spectral interferences in elemental and isotopic analysis using inductively coupled plasma mass spectrometry. In this study, the behavior of ArM⁺ ions for vanadium, manganese, cobalt, and copper was experimentally investigated as a function of high-frequency plasma power and transporting argon flow rate. The behavior of ArV⁺ and ArCo⁺ ions was theoretically studied using thermodynamic simulation with changes in plasma temperature, transporting argon flow, concentration of the element M, acid type, and concentration of sodium as an easily ionizable element in the studied solution. General trends in the ratios of experimental intensities and theoretical particle concentrations ArM⁺/M⁺ were observed with changes in operational parameters. The form of the experimental and theoretical dependencies was consistent: an increase in the ArM⁺/M⁺ ratio with a decrease in plasma temperature.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 5","pages":"864 - 876"},"PeriodicalIF":1.1,"publicationDate":"2025-06-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145143720","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}