Journal of Analytical Chemistry最新文献

{"title":"Development and Validation of a Derivatization-Based Spectrophotometric Procedure for Pregabalin Determination","authors":"Burak Bayrak,&nbsp;Yucel Kadioglu,&nbsp;Mehmet Serdar Gultekin,&nbsp;Bilal Yılmaz,&nbsp;Amine Sena Aydin","doi":"10.1134/S1061934826700723","DOIUrl":"10.1134/S1061934826700723","url":null,"abstract":"<p>In this study, a sensitive, rapid, economical, and simple derivatization-based spectrophotometric procedure was developed and validated for the determination of pregabalin in bulk substance and pharmaceutical formulations. The procedure is based on the formation of a chromogenic imine derivative through the reaction of the primary amine group of pregabalin with 2-naphthaldehyde in a basic medium. Experimental design methodology was applied to screen and optimize the critical reaction parameters, including K₂CO₃ concentration, temperature, and ethanol volume. A central composite design was employed to evaluate factor effects and to establish the optimal derivatization conditions. After derivatization, absorbance measurements were performed at 228 nm in the UV spectrum and at 236 nm for the first-derivative spectrophotometric mode. The procedure showed linearity in the concentration range of 2–30 µg/mL for the direct UV measurement and 2–50 µg/mL for the first-derivative measurement, with coefficients of determination greater than 0.999. The analytical performance of the procedure was validated according to ICH Q2(R1) guidelines with respect to linearity, precision, accuracy, limits of detection and quantification, and stability. The results demonstrate that the proposed derivatization-based spectrophotometric procedure provides a reliable, reproducible, and cost-effective alternative for the quantitative analysis of pregabalin in pharmaceutical quality control laboratories.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"1405 - 1413"},"PeriodicalIF":1.5,"publicationDate":"2026-08-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148807376","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":"Luminescence–Colorimetric Determination of Adrenaline Using Carbon Nanodots","authors":"M. M. Ivanova,&nbsp;K. V. Stepanova,&nbsp;A. A. Vasilyeva,&nbsp;M. V. Matiash,&nbsp;V. V. Apyari,&nbsp;S. V. Maksimov,&nbsp;S. G. Dmitrienko","doi":"10.1134/S1061934826700681","DOIUrl":"10.1134/S1061934826700681","url":null,"abstract":"<p>Carbon nanodots (<b>CND</b>s) of an average size of 2.7 ± 0.1 nm, exhibiting intense luminescence at 465 nm upon irradiation with a wavelength of 365 nm were synthesized from citric acid using the pyrolytic method. It was shown that, in the presence of the oxidized form of adrenaline, absorbing light at 365 nm, a noticeable quenching of the luminescence of CNDs was observed, which can be used for the luminescence determination of adrenaline. As CNDs are characterized by luminescence in the visible spectral region, both visual and colorimetric (using a camera and a smartphone camera) determination of adrenaline is possible; the achieved limit of detection is 0.8 μM, which is comparable with to limits of detection of the described versions of instrumental determination. The proposed colorimetric methods for determining adrenaline can be used for the quality control of medicinal products.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"1354 - 1363"},"PeriodicalIF":1.5,"publicationDate":"2026-08-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148807422","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":"Assessment of Eco-Whiteness and Green Analytical Profiles of Microfluidic Paper Analytical Device and Spectrophotometric Methods for the Determination of Olanzapine in Pharmaceuticals","authors":"Zahraa M. Abbas,&nbsp;Mohammad K. Hammood","doi":"10.1134/S1061934825604414","DOIUrl":"10.1134/S1061934825604414","url":null,"abstract":"<p>This study presents the development and validation of three analytical methods for estimating the antipsychotic drug olanzapine (<b>OLP</b>) in pharmaceutical preparations. The first method is a conventional spectrophotometric technique based on a redox reaction between olanzapine and ferric chloride, followed by complexation with potassium ferricyanide, which produces Prussian blue with an absorption peak at 717 nm. In parallel, two microfluidic paper analytical device (<b>µPAD</b>) platforms were fabricated using wax printing with two different designs, enabling miniaturized, low-cost, and environmentally friendly modifications of the same colorimetric reaction. The spectrophotometric method (Method I) showed excellent linearity within the range of 0.1–10 μg/mL, with a limit of detection (<b>LOD</b>) of 0.03 μg/mL. The µPAD methods (Methods II and III) showed linear ranges of 0.5–5 and 1–5 μg/mL, with LODs of 0.3 and 0.26 μg/mL, respectively. All methods demonstrated satisfactory precision (RSD &lt; 2%). The greenness of the methods was evaluated using various assessment tools, including the analytical eco-scale, ChlorTox, analytical GREEnness (<b>AGREE</b>) metrics, and AGREEprep. The results showed an excellent greenness profile, and white analytical chemistry was also evaluated by the Red-Green-Blue 12 algorithm, which gave excellent whiteness scores above 85 for all methods. The proposed µPAD systems offer an environmentally friendly, portable, and highly reproducible alternative for point-of-care or on-site drug analysis. The results of this investigation showed that OLP in dosage forms may be reliably assessed using the suggested methods.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"1414 - 1427"},"PeriodicalIF":1.5,"publicationDate":"2026-08-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148807368","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":"Fluorine Determination via Megahertz and Gigahertz Inductively Coupled Plasma Mass Spectrometry: A Review","authors":"A. A. Pupyshev","doi":"10.1134/S1061934826700644","DOIUrl":"10.1134/S1061934826700644","url":null,"abstract":"<p>This review summarizes published studies on the mass spectrometric determination of fluorine using conventional megahertz inductively coupled plasma and microwave (gigahertz) inductively coupled plasma. The formation of F⁺, F^–, BaF⁺, and other fluorine-containing polyatomic ions in high-temperature inductively coupled plasma is examined, along with the analytical performance achieved for fluorine determination using different analytical approaches. Particular attention is given to the selection of chemical reagents for the mass spectrometric determination of fluorine via polyatomic ions, as well as to the investigation of the effects of operating parameters on the BaF⁺ ion signal. Isobaric spectral interferences encountered during fluorine determination and the methods used to eliminate them are discussed. The feasibility of fluorine determination using various fluorine-containing polyatomic ions formed by chemical ionization in the cold afterglow regions of megahertz inductively coupled plasma is demonstrated. Publications on the mass spectrometric determination of fluorine using microwave plasma and various chemical ionization strategies for the formation of fluorine-containing polyatomic ions are also reviewed. Conclusions and recommendations based on the reviewed publications are presented.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"1302 - 1320"},"PeriodicalIF":1.5,"publicationDate":"2026-08-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148807375","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 Self-Assembled Nanocomposite of Magnetic Graphene Oxide Modified Macroporous Resin for Sensitive Determination of Fluoroquinolones in Environment Water Samples","authors":"Ou Sha,&nbsp;Yunfan Wu,&nbsp;Yuan Xu,&nbsp;Yang Yao,&nbsp;Zhaoyun Wang,&nbsp;Shaoyuan Guo,&nbsp;Chao Wang","doi":"10.1134/S1061934824604559","DOIUrl":"10.1134/S1061934824604559","url":null,"abstract":"<p>In this study, a novel magnetic graphene oxide modified macroporous resin was successfully synthesized via a mechanochemical method and employed as the adsorbent for magnetic solid-phase extraction coupled with high-performance liquid chromatography-fluorescence detection for the determination of trace fluoroquinolones in environmental water samples. Moreover, the magnetic nanocomposite prepared was characterized and the parameters of magnetic solid-phase extraction were optimized. The results indicated that the adsorption mechanism of Fe₃O₄@GO@MR toward FQs was more consistent with the quasi-second-order kinetic model, with a maximum adsorption capacity of 25.8–37.5 mg/g. Under optimal conditions, the limits of detection and quantification were 4 × 10^–4–4 × 10^–2 mg/L and 2 × 10^–3–9 × 10^–2 mg/L, respectively, with good linearity in the range from 5 × 10^–4 to 1 mg/L (<i>R</i>² ≥ 0.9991). The average recovery was between 93.6% and 100.1% with relative standard deviation less than 5.5%. The established method was applied to quantify fluoroquinolones in actual water samples with good accuracy and reliability, providing a serviceable perspective for expanding the trace analysis and detection of fluoroquinolones in complex samples.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"1394 - 1404"},"PeriodicalIF":1.5,"publicationDate":"2026-08-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148807491","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-Free Urinary Iodine Determination via Iodide-Electron Shuttle Catalysis: A Rapid Kinetic Method on Automated Biochemical Analyzers","authors":"Na Li,&nbsp;Huilin Shao,&nbsp;Yongxia Huang,&nbsp;Bingyuan Su,&nbsp;Minshan Wu,&nbsp;Yaping Zhang,&nbsp;Shuying Huang","doi":"10.1134/S1061934825602518","DOIUrl":"10.1134/S1061934825602518","url":null,"abstract":"<p>A novel arsenic-free method for the determination of iodine in urine was developed using a cerium(IV)−Ferroin catalytic reaction combined with an automated biochemistry analyzer. The method was based on the oxidation of the Ferroin reagent by cerium(IV) ions in an acidic medium, followed by reduction with hydrazine hydrochloride. Iodide ions catalyzed the reaction, and the absorbance was measured using an automated biochemistry analyzer. A quadratic relationship between iodine concentration (<i>c</i>, μg/L) and absorbance (<i>A</i>) was observed within the range of 0–400 μg/L and was described by the regression equation <i>c</i> = <i>aA</i>² + <i>bA</i> + <i>d</i>, with a coefficient of correleation (<i>r</i>) greater than 0.999. The method exhibited high sensitivity, with a limit of detection for urinary iodine of 3.6 μg/L. Excellent precision was achieved, with an intra-assay coefficient of variation (<b>CV</b>) of ≤3.0% and inter-assay CVs of &lt;3% for low, medium, and high iodine concentration standards. Accuracy was confirmed by an average recovery rate of 98.3% in spiked samples. The results obtained from the simultaneous determination of 40 urine samples using this method were highly consistent with those obtained by the standard arsenic-cerium catalytic spectrophotometry method, demonstrating good reliability and accuracy for urinary iodine determination. Owing to its high sensitivity, precision, accuracy, and rapid analysis performance, the proposed arsenic-free method was considered suitable for large-scale monitoring of iodine deficiency disorders and showed broad potential for application in urinary iodine detection while ensuring improved environmental and occupational safety.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"1236 - 1243"},"PeriodicalIF":1.5,"publicationDate":"2026-08-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148652195","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 Capabilities of Fluorescence Polarization Immunoassay and Amperometric Tyrosinase Immunosensors in the Determination of Chloramphenicol","authors":"R. M. Beilinson,&nbsp;A. A. Yavisheva,&nbsp;I. Tsui,&nbsp;Q. Yang,&nbsp;A. A. Kuksenok,&nbsp;E. P. Medyantseva,&nbsp;N. Yu. Ilyicheva,&nbsp;R. R. Zairov,&nbsp;A. P. Dovzhenko,&nbsp;S. A. Eremin","doi":"10.1134/S1061934826700590","DOIUrl":"10.1134/S1061934826700590","url":null,"abstract":"<p>A version of competitive fluorescence polarization immunoassay (<b>FPIA</b>) and an amperometric immunosensor with a tyrosinase tracer have been developed for the sensitive and selective determination of the chloramphenicol antibiotic. In the development of FPIA for the determination of chloramphenicol, a green fluorescent complex of terbium(III) was first used as a tracer, which changed emission in the green spectral region with a maximum at 545 nm. The competitive binding of the substance to be determined with a limited number of binding sites of specific antibodies (<b>ABs</b>) in using this tracer ensured the determination of chloramphenicol in the linear range of the calibration dependence of fluorescence polarization on the analyte concentration in the range 1 × 10^–11–1 × 10^–7 M, LOD = 9 × 10^–12 M. To ensure the maximum value of the analytical signal, tracer dilution was selected at 1 : 10 and antibody dilution, at 1 : 25. The optimal incubation time for the tracer–antibody immune complex was 5 min. Tyrosinase enzyme was used as a tracer in the development of an amperometric enzyme-linked immunosorbent assay (<b>ELISA</b>) sensor for the detection of chloramphenicol. The work of this sensor is based on a combination of immunochemical, enzymatic, and electrochemical reactions, leading to “quasi-inhibition” effects. The developed amperometric immunosensor for the determination of chloramphenicol ensured its determination in a narrower concentration range from 1 × 10^–9 to 1 × 10^–6 M, LOD = 8 × 10^–10 M. The conditions of analysis were as follows: AB dilution of 1 : 200 and the duration of an analysis 10 min. The developed versions for the determination of chloramphenicol were tested in analyses of food products (milk). The error of the determination dis not exceed 0.059.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"1190 - 1198"},"PeriodicalIF":1.5,"publicationDate":"2026-08-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148652241","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":"Formation of Structured Oligonucleotide Clusters in High-Throughput DNA Sequencing with Fluorescence Detection","authors":"A. L. Bulyanitsa,&nbsp;D. A. Belov,&nbsp;I. V. Zarutsky,&nbsp;V. V. Manoilov,&nbsp;Ya. I. Alekseev,&nbsp;A. A. Evstrapov","doi":"10.1134/S1061934826700607","DOIUrl":"10.1134/S1061934826700607","url":null,"abstract":"<p>The article presents solutions corresponding to protocols for the formation of structured clusters of DNA fragments in filling a flow cell for the high-throughput DNA sequencing taking into account various integral quality indicators. Conditions for implementing a possibility of the detection of a polyclonal cluster were investigated. Recommendations are given for choosing an algorithm of cluster formation depending on the relative importance of the following characteristics: minimization of the number of microwells, minimization of the fraction of “lost” DNA fragments and/or used microwells, maximization of the speed of analysis, and various combinations of the specified requirements.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"1199 - 1203"},"PeriodicalIF":1.5,"publicationDate":"2026-08-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148652243","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":"Establishment of Preparation Conditions for Silica Monolithic Rods Using the Sol-Gel Method and a Study on Their Characteristics","authors":"Chol Hyon Kim,&nbsp;Jong Nam Kim,&nbsp;Mi Yang Kim,&nbsp;Il Chon Ri,&nbsp;Chung Song Choe","doi":"10.1134/S1061934825604098","DOIUrl":"10.1134/S1061934825604098","url":null,"abstract":"<p>Silica monolithic rods are inorganic materials used as packing materials in monolithic separation columns, a global trend in material separation, particularly in high-performance liquid chromatography (<b>HPLC</b>). Unlike the previously widely used separation columns with spherical silica packing, these monolithic columns suffer from various problems, including shrinkage, deformation, and cracking during the preparation of rods, limiting their application. This paper describes the development of a new type of silica monolithic rod that can significantly shorten analysis time while maintaining high separation efficiency in HPLC.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"1250 - 1260"},"PeriodicalIF":1.5,"publicationDate":"2026-08-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148652269","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":"Colorometric Determination of Catecholamines Using Silica Nanodots","authors":"A. A. Vasilyeva,&nbsp;M. V. Matiash,&nbsp;V. V. Apyari,&nbsp;S. V. Maksimov,&nbsp;S. G. Dmitrienko","doi":"10.1134/S1061934826700504","DOIUrl":"10.1134/S1061934826700504","url":null,"abstract":"<p>The possibility of colorimetric determination of catecholamines using silica nanodots with a digital camera and smartphone is demonstrated. A lamp and a diode with emission wavelengths of 395 and 360 nm, respectively, are used as excitation sources. Color coordinates in the RGB, CMYK, and Lab systems, as well as some combinations thereof, are used as analytical signals. It is demonstrated that using a lamp as a source of ultraviolet radiation allows for achieving the best detection limits for all three catecholamines: 7, 0.1, and 1 μM when using a camera, and 12, 0.3, and 5 μM for dopamine, norepinephrine, and epinephrine, respectively, when using a smartphone. The data are obtained for the Euclidean distance analytical signal in the CMYK system. Using a camera and other color coordinate combinations as analytical signals can reduce the detection limits to 0.1 μM for epinephrine (coordinate combination L-a + b) and to 1 μM for dopamine (coordinate combination R + G + B). The pharmaceuticals “Dopamine-Ferein” (ZAO “Bryntsalov-A,” Russia), “Adrenaline Hydrochloride—Vial” (VIAL, China), and “Noradrenaline” (ZAO “EcoPharmPlus,” Russia) are analyzed. The results of colorimetric determination are in good agreement with the luminescence and HPLC analysis data.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"81 :","pages":"1101 - 1109"},"PeriodicalIF":1.5,"publicationDate":"2026-08-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148652192","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}