Journal of Analytical Chemistry最新文献

{"title":"Eco-Friendly Method for the Determination of Lanreotide in Human Plasma Using Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry: Assessment of Greenness using the Analytical Greenness Metric Tool, Analytical Eco-Scale, and Green Analytical Procedure Index","authors":"Priyanka A. Shah,&nbsp;Primal Sharma,&nbsp;Mallika Sanyal,&nbsp;Gh. Ali,&nbsp;Pranav S. Shrivastav","doi":"10.1134/S106193482470196X","DOIUrl":"10.1134/S106193482470196X","url":null,"abstract":"<p>An efficient, sensitive, and eco-friendly ultra-high-performance liquid chromatography-tandem mass spectrometry method was developed to determine lanreotide in human plasma. The extraction of lanreotide and lanreotide-d8 from 300 µL human plasma using an Oasis^® HLB 96-well µElution Plate yielded a consistent mean percentage of recoveries of 73.2%. The extracts were analyzed on a Peptide HSS T3 column under gradient-based separation conditions with a flow rate of 0.3 mL/min. The mobile phase consisted of 0.1% formic acid in water and acetonitrile. The detection was performed using a tandem mass spectrometer in positive ionization mode. Multiple reaction monitoring was used to analyze doubly charged precursor ions for lanreotide (<i>m</i>/<i>z</i> 548.8 → 170.0) and lanreotide-d8 (<i>m</i>/<i>z</i> 552.6 → 170.1). The method demonstrated good linearity over a concentration range of 0.1–20 ng/mL with a correlation coefficient greater than 0.997. The intra- and inter-batch precision (coefficient of variation) ranged from 1.5 to 7.4%, and the accuracy was 94.3–103.6%. The lanreotide-d8-normalized matrix factors ranged from 0.976 to 1.021. The analyte demonstrated sufficient stability under different analytical conditions. Further, the greenness of the developed method was assessed by the Analytical Greenness metric tool, Analytical Eco-Scale, and Green Analytical Procedure Index.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 3","pages":"490 - 500"},"PeriodicalIF":1.0,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143913808","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 Cadmium and Zinc in Soil Samples Using Magnetic Field-Assisted Solution Cathode Glow Discharge","authors":"Quanfang Lu,&nbsp;Xiaoxia Hao,&nbsp;Jie Yu,&nbsp;Kai Wang,&nbsp;Xuehe Li","doi":"10.1134/S1061934824701946","DOIUrl":"10.1134/S1061934824701946","url":null,"abstract":"<p>A magnetic field-assisted solution cathode glow discharge (<b>MF-SCGD</b>) was established and then applied for the detection of Cd and Zn in soil samples. In order to reveal the signal enhancement mechanism of the magnetic field, the influence of the magnetic field strength on plasma parameters, such as electron temperature and electron density, was investigated. The results showed that adding a 0.5 T magnetic field significantly reduces the red-hot degree of the Pt needle, decreases the volume of the plasma torch, extends the lifespan of the Pt needle, and widens the application range of voltage. The optimal operating parameters of MF-SCGD were identified as a 0.5 T magnetic field, 680 V discharge voltage, 3.2 mL/min solution flow rate, and pH 1.0 HNO₃ as the supporting electrolyte. Under optimal conditions, the intensities of Cd and Zn signals increased by 1.7 and 1.8 times, respectively. The limits of detection were 9.1 μg/L for Cd and 12.0 μg/L for Zn. After adding a 0.5 T magnetic field, electron temperature slightly decreased while electron density increased. The plasma parameter β was found to be less than 1, indicating that signal intensity enhancement is due to magnetic confinement. The analysis results of Cd and Zn in certified reference materials and two soil samples are consistent with the certified standard and verified values obtained <i>via</i> inductively coupled plasma optical emission spectroscopy. MF-SCGD is a promising technique with a compact instrument, low cost, low power consumption, and high discharge stability.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 3","pages":"467 - 479"},"PeriodicalIF":1.0,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143913854","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":"Chemical Analysis on the Way to a Mass Consumer: Solutions for Food Quality Control","authors":"V. V. Apyari,&nbsp;Yu. A. Zolotov,&nbsp;S. G. Dmitrienko,&nbsp;A. A. Furletov,&nbsp;T. I. Tikhomirova","doi":"10.1134/S1061934824701867","DOIUrl":"10.1134/S1061934824701867","url":null,"abstract":"<p>A pronounced trend in present-day analytical chemistry is increasing availability of chemical analysis for a mass consumer. To date, a large number of serial test kits for semi-quantitative analysis and a series of devices for assessing the compliance of individual parameters of an analyzed sample with the required standards have appeared. The review systematizes and discusses the main solutions currently available in this area for food analysis and reflects its current state. According to the authors opinion, the concept of the availability of a particular accessory is largely determined by its presence on the market and the acceptance of its cost to an individual consumer; therefore, the review focuses on commercialized analytical tools costing mainly up to 100 thousand rubles. Relatively inexpensive and easy-to-use test tools; portable electrochemical, spectroscopic, refractometric, and ultrasonic systems; as well as electronic nose systems for chemical analysis are considered and their main characteristics and approximate cost are given. Assumptions are made about the prospects for the further development of chemical analysis tools available to a mass consumer.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 3","pages":"385 - 401"},"PeriodicalIF":1.0,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143913864","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":"Room-Temperature Phosphorescence of Organic Compounds in Diverse Supramolecular Matrix Systems","authors":"G. I. Romanovskaya","doi":"10.1134/S1061934824701879","DOIUrl":"10.1134/S1061934824701879","url":null,"abstract":"<p>The review considers the works of Russian and foreign researchers from 1999 to 2024 focused on the development of novel methods for observing phosphorescence in natural and synthesized chemical compounds at room temperature in the presence of various supramolecular structures and nanostructured molecular assemblies. The analysis of the research findings demonstrates that room-temperature phosphorescence in the studied systems is due to the formation of either self-organizing supramolecular structures with tunable spectral properties or nanostructured molecular assemblies. These structures ensure rigidity, necessary for the minimization of collisions that suppress phosphorescence and prevent the nonradiative deactivation of the triplet state of luminophores in liquid and solid solutions, as well as on nanoparticle surfaces.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 3","pages":"402 - 410"},"PeriodicalIF":1.0,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143913865","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":"Unified Theoretical and Experimental Bases of Micro-Thermal Field-Flow Fractionation","authors":"J. Janča,&nbsp;I. A. Ananieva","doi":"10.1134/S1061934824701892","DOIUrl":"10.1134/S1061934824701892","url":null,"abstract":"<p>The Micro-Thermal Field-Flow Fractionation (<b>Micro-TFFF</b>) was proposed and continuously developed for the analytical separations of macromolecular and particulate species of synthetic, natural and biological origin. The progress in theory of the separation mechanisms of Micro-TFFF inspired the improvement of the experimental methodology and instrumentation. On the other hand, the important progress in construction of more powerful apparatuses permitted to attain the performance of analytical separations close to the predicted theoretical limits. Surface properties of colloidal particles, exposed to the temperature gradient, influence fundamentally their migration. The spherical particles of identical size but of different surface properties migrate in temperature gradient differently. The shape and surface topographical heterogeneity of the particles also distinguish their thermal diffusion. It was anticipated and theoretically calculated that the separations of the colloidal particles based on the mentioned particular differences could be possible by using Micro-TFFF. The theoretical conclusions were confirmed by real separations of various particulate species including living bacteria cells.|</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 3","pages":"423 - 431"},"PeriodicalIF":1.0,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143913802","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":"Detection of Explosives: A Comparison of Analytical and Operational Characteristics of Mass Spectrometers and Ion Mobility Spectrometers","authors":"T. I. Buryakov,&nbsp;I. A. Buryakov","doi":"10.1134/S1061934824701880","DOIUrl":"10.1134/S1061934824701880","url":null,"abstract":"<p>The main analytical and operational characteristics of stationary (laboratory) and portable (handheld) mass spectrometers and ion mobility spectrometers for detecting traces and vapors of explosives were compared. The limit of detection, the setting time (speed of response), the (linear) range of detectable substance content in samples, the resolution, and the cost of the specified instruments were considered. The requirements for the performance and reliability of detection, maintenance, and the qualifications of service and maintenance personnel were discussed. Promising areas for further improvement of these instruments were listed.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 3","pages":"411 - 422"},"PeriodicalIF":1.0,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143913806","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 Effect of X-Ray Radiation on the Structural Characteristics of Bovine Serum Albumin Protein Using High-Resolution Liquid Chromatography−Mass Spectrometry","authors":"A. V. Brown,&nbsp;U. A. Bliznyuk,&nbsp;P. Yu. Borshchegovskaya,&nbsp;V. S. Ipatova,&nbsp;A. P. Chernyaev,&nbsp;I. A. Ananieva,&nbsp;I. A. Rodin","doi":"10.1134/S1061934824701983","DOIUrl":"10.1134/S1061934824701983","url":null,"abstract":"<p>A method for assessing changes in the structural characteristics of the bovine serum albumin (<b>BSA</b>) protein in an aqueous solution as a result of exposure to ionizing radiation is developed and tested. The method consists in identifying unique peptides of the protein domain structures, as well as in establishing modifications of the amino acid sequence using high-resolution liquid chromatography–mass spectrometry. A BSA solution is irradiated by X-rays from a tube of a voltage of 80 kV and average current of 1 mA, the dose rate is 2 Gy/s. The absorbed dose in the sample volume is estimated by the ferrosulfate dosimetry method. An aqueous solution of BSA is irradiated at doses of 0.1, 0.5, 1, 2, 4, and 8 kGy, after which the amount of protein molecules in the solution is quantitatively estimated and the structural integrity of the native form of the protein is analyzed, as well as amino acid modifications in the BSA sequence as a result of exposure to radiation are established. For a more in-depth analysis, the cysteine–cysteine disulfide bonds of BSA are reduced, followed by the alkylation of the resulting thiol residues with bromoacetic acid amide. The enzymatic hydrolysis of BSA is carried out with the addition of a trypsin solution. The resulting samples are analyzed by high-resolution liquid chromatography–mass spectrometry with high-resolution tandem mass spectrometric detection. Next, the change in the number of intact protein molecules is estimated by determining unique peptides corresponding to each of the three domains forming the amino acid sequence of BSA. Taking into account the optimization of the detection conditions for the three domains as markers of the active form of BSA, the limit of detection for each peptide is calculated. The developed approach makes it possible to establish a change in the natural conformation of the bovine serum albumin protein (its denaturation) in water samples as a result of exposure to ionizing radiation at doses of 4−8 kGy at an average power of 2 Gy/s.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 3","pages":"515 - 525"},"PeriodicalIF":1.0,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143913810","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":"Gold Nanoparticles Electrochemically Deposited on Carbon Nanomaterials and Thiacalixarenes in Immunosensors for Determining Tricyclic Antidepressants","authors":"D. V. Brusnitsyn,&nbsp;A. N. Ramazanova,&nbsp;E. P. Medyantseva,&nbsp;E. R. Ramazanova,&nbsp;A. V. Prytkova,&nbsp;E. R. Karimova,&nbsp;M. A. Ziganshin,&nbsp;V. A. Burilov,&nbsp;E. G. Makarov,&nbsp;T. L. Khamidullin","doi":"10.1134/S1061934824702010","DOIUrl":"10.1134/S1061934824702010","url":null,"abstract":"<p>Composite materials based on gold nanoparticles electrochemically deposited on a carbon substrate of functionalized graphene oxide, reduced graphene oxide, and carbon nanotube paper in the cyclic voltammetry and chronoamperometry mode are proposed. Screening of composite materials by atomic force microscopy, electrochemical impedance spectroscopy, and voltammetry made it possible to select the best ones as modifiers of planar electrodes, on the basis of which highly sensitive immunosensors are developed. For the best amperometric immunosensors based on a combination of carbon paper, amino(thia)calix[4]arene, and gold nanoparticles, the range of working concentrations for the determination of amitriptyline and desipramine is 1 × 10^–9–1 × 10^–4 M, the limit of quantification is (4–6) × 10^–10 M. Amitriptyline and desipramine are determined by amperometric immunosensors in pharmaceutical preparations with the relative standard deviation no more than 4%. A Comparison of the results of the determination of tricyclic antidepressants in human urine by immunosensors and fluorescence polarization immunoassay with a relative standard deviation no more than 8.5% indicates the accuracy and repeatability of the results obtained.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 3","pages":"553 - 563"},"PeriodicalIF":1.0,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143913827","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":"Approximation of the Results of Analysis of Thermally Unstable Compounds by Gas Chromatography Using Logistic Regression","authors":"I. G. Zenkevich,&nbsp;T. A. Kornilova","doi":"10.1134/S1061934824701995","DOIUrl":"10.1134/S1061934824701995","url":null,"abstract":"<p>The decomposition of thermally unstable components in chromatograph sample injectors often occurs during gas chromatographic analysis. However, variations in the absolute areas of gas chromatographic peaks at different injector temperatures generally do not reveal this decomposition. This is due to the area discrimination effects, which are typical for samples introduced into capillary columns with flow splitting. This problem can be solved using relative peak areas, calculated in relation to thermally stable compounds. The relationships between the relative peak areas of unstable analytes and temperature (decreasing) and between those of their decomposition products and temperature (increasing) are characterized by the existence of two limits. Low-temperature limits correspond to the actual concentration of unstable compounds or their decomposition products in the samples, while high-temperature limits reflect the composition of samples under the hypothetical condition of the complete transformation of such analytes. These relationships can be approximated using the logistic regression equation, also known as sigmoidal approximation or Boltzmann approximation. To evaluate the applicability of logistic regression to processing the results of a gas chromatographic analysis of thermally unstable compounds, this study examines the potential for approximating the temperature dependence of ethyl diazoacetate peak areas in various solvents. The results confirm that the gas chromatographic analysis of this ester, as well as likely other diazocarbonyl compounds, can be performed without their significant decomposition at injector temperatures up to 200°C. The thermal decomposition of ethyl diazoacetate in its solutions with aliphatic alcohols is accompanied by the formation of ethyl esters of alkoxyacetic acids. These are products of the insertion of the intermediate ethoxycarbonyl carbene into O−H bonds of alcohols. A characteristic feature of logistic regression, specifically the argument value corresponding to the mean function value, indicates that the temperatures for the analyte’s half-life and the time of the formation of half of products are equal. This relationship allows these processes to be correlated with each other. A slight modification of the proposed method (adding a point corresponding to the zero peak area at a hypothetical high injector temperature) enables its application to the characterization of compounds with half-life temperatures above 300°C. This variation was used to evaluate the thermal stability or instability of halogen-substituted alkyl- and cycloalkyl-aromatic hydrocarbons under the conditions of gas chromatographic analysis.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 3","pages":"526 - 539"},"PeriodicalIF":1.0,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143913852","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":"All-Solid-State Potentiometric Sensor Based on Carbon Paste Composite for the Selective Determination of Iodide Ions","authors":"Semra Yilmaz,&nbsp;Fatih Coldur","doi":"10.1134/S1061934824702009","DOIUrl":"10.1134/S1061934824702009","url":null,"abstract":"<p>In the current study, a potentiometric all-solid-state composite ion-selective electrode for the determination of iodide ions is described. The synthesized salicylaldehyde thiosemicarbazone-mercury(II) complex (<b>SATSC-Hg(II)</b>) (1 : 1) was applied as the electroactive material in the electrode structure. Various composite ion-selective electrodes were prepared with different compositions, including SATSC-Hg(II), graphite, multi-walled carbon nanotubes (<b>MWCNTs</b>), ionic additives, and some mediators (various plasticizers or paraffin oil) to identify the most effective composite sensing layer composition exhibiting satisfactory potentiometric characteristics. The sensing layer composition consisting of 10 mg SATSC-Hg(II) complex, 26 mg dioctyl phthalate plasticizer, 5 mg MWCNTs, 4 mg methyltrioctylammonium chloride, and 65 mg graphite yielded the most favorable potentiometric performance properties. The electrode demonstrated a linear operating range of 1.0 × 10^–5 to 0.1 M, a slope value of 55.2 ± 0.2 mV/decade, a detection limit of (9.0 ± 0.2) × 10^–6 M, a pH operating range of 4–8, and a response time of approximately 60 s. The proposed electrode also displayed reproducible, stable, and selective potentiometric response to iodide ions. The analytical application of the electrode involved its use as an indicator electrode in the titration of iodide ions in synthetic solutions and for the determination of KI content in a pharmaceutical used for the treatment of goiter by the multiple standard addition method. Compared to polymer membrane electrodes, the renewability and reusability of the sensing surface of the proposed electrode, its suitability for miniaturization, and its robust structure offer significant advantages.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 3","pages":"540 - 552"},"PeriodicalIF":1.0,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143913853","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}