{"title":"Development of an Eco-Friendly Liquid Chromatography Method for the Separation and Trace Determination of Caffeine in Beverages, Pharmaceuticals, and Environmental Water Samples Utilizing High-Temperature and Superheated Water: A Greenness Assessment","authors":"Lateefa A. Al-Khateeb, Fatimah A. Dahas","doi":"10.1134/S1061934825700121","DOIUrl":"10.1134/S1061934825700121","url":null,"abstract":"<p>The retention behavior of the central nervous system stimulant caffeine (<b>CAF</b>) on the thermally stable Zir-Chrom-PBD column (5 μm, 150 × 4.6 mm) was investigated thermodynamically at various elevated temperatures utilizing high-temperature liquid chromatography (<b>HTLC</b>). The HTLC method was optimized for CAF analysis. The determination was performed using pure water or 20% acetonitrile in water as the mobile phase.The lower limit of detection for CAF was found to be 0.008 mg/mL, whereas the limit of quantification was 0.026 mg/mL. The developed HTLC method is the first HTLC method for this compound and has been used for multiple applications. It was applied for the assay of CAF in tablets and energy drinks, with acceptable mean recoveries ranging from 99.7 ± 0.3 to 100.0 ± 0.2% and 90.9 ± 1.9 to 103.6 ± 2.1%, respectively. Furthermore, the HTLC method was applied for monitoring of CAF in wastewater and groundwater. Multi-walled carbon nanotubes (<b>MWCNT</b>s) were applied for the efficient removal of CAF from water, and a mechanism of interaction between CAF and the MWCNTs was proposed. The method greenness was positively evaluated using two tools: the Analytical GREEnness metric and the Green Analytical Procedure Index.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 4","pages":"693 - 706"},"PeriodicalIF":1.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949461","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":"Quantification of the Anticancer Drug Avapritinib in Human Plasma Using 2,2-Dihydroxyindane-1,3-Dione: Application to a Pharmacokinetic Study","authors":"Baher I. Salman","doi":"10.1134/S1061934825700108","DOIUrl":"10.1134/S1061934825700108","url":null,"abstract":"<p>The study examined the effectiveness of 2,2-dihydroxyindane-1,3-dione, commonly utilized as a derivatizing reagent for quantifying avapritinib (<b>AVB</b>) in pure form, pharmaceutical dosage formulations, and human plasma samples. In 2020, the United States Food and Drug Administration (<b>US</b> <b>FDA</b>) approved AVB, marking it as the inaugural precision therapy for individuals suffering from unresectable or metastatic gastrointestinal stromal tumors and advanced systemic mastocytosis. Therefore, adjusting the AVB dose is essential for drug monitoring. Hence, the described spectrofluorimetric technique relies on a condensation reaction involving 2,2-dihydroxyindane-1,3-dione and the primary amine group found in AVB in the presence of phenylacetaldehyde. This reaction yields a highly fluorescent compound detectable at 468 nm (excitation wavelength of 395 nm). The calibration curve was established within a range of 0.4–4.0 µg/mL, demonstrating an excellent correlation coefficient of 0.9993 and a lower limit of quantification of 0.10 µg/mL. The methodology proved effective in estimating AVB in spiked plasma samples and assessing content uniformity. The research protocol was established and validated through bioanalytical methods by the ICH and US FDA guidelines. Additionally, this approach was employed to verify the drug concentration in each tablet, achieving a high recovery rate of 101.37% during the content uniformity test. This method was designed for pharmacokinetic analysis and easily applied in clinical laboratories.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 4","pages":"675 - 683"},"PeriodicalIF":1.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949483","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":"State-of-the-Art Technologies in Explosives Detection","authors":"I. A. Buryakov, T. I. Buryakov","doi":"10.1134/S1061934825700029","DOIUrl":"10.1134/S1061934825700029","url":null,"abstract":"<p>This review substantiated the list of explosive substances and their components subject to control. Typical objects of detection by instrumental methods of chemical analysis—trace amounts of explosives on various surfaces or explosive vapors in the air as signs of the presence of explosive devices or explosive charges—were described. Based on these descriptions, requirements for the explosives detectors in use were formulated. An assessment and qualitative comparison of analytical and operational characteristics of devices based on remote methods of laser spectroscopy and also devices based on sampling, sample preparation, and analysis by ion mobility spectrometry, colorimetry with the use of reagents for color reactions, mass spectrometry, high-speed gas chromatography, gas chromatography—mass spectrometry, high-performance liquid chromatography, and sensor methods (optical (chemical), electrical, electrochemical, thermometric, and mass-sensitive methods) were carried out. The main directions in the development of instrumental analytical technologies for explosives detection were listed.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 4","pages":"591 - 607"},"PeriodicalIF":1.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949583","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":"Simultaneous Determination of Chiral Amino Acid Enantiomers by Liquid Chromatography–Mass Spectrometry Using (S)-2,5-Dioxypyrrolidine-1-yl-(5-(4-Methylpiperazin-1-yl)-2,4-Dinitrophenyl) Pyrrolidine-2-Carboxylate as a Chiral Derivatizing Reagent","authors":"Biao Jin, Zhiyin Jin, Dongri Jin","doi":"10.1134/S1061934825700145","DOIUrl":"10.1134/S1061934825700145","url":null,"abstract":"<p>(S)-2,5-Dioxypyrrolidine-1-yl-(5-(4-methylpiperazin-1-yl)-2,4-dinitrophenyl) pyrrolidine-2-carboxylate (<b>PPZ-Pro-NHS</b>) was used as the reagent for chiral derivatization to distinguish between amino acid enantiomers. PPZ-Pro-NHS, synthesized from (S)-1-(5-(4-methylpiperazin-1-yl)-2,4-dinitrophenyl) pyrrolidine-2-carboxylic acid, reacted with chiral amines under mild conditions to yield the corresponding organic derivatives. The optimal conditions for derivatization using PPZ-Pro-NHS were 25°C and 40 min in a medium containing triethylamine. A simple liquid chromatography–mass spectrometry (<b>LC</b>−<b>MS</b>) method was developed to separate chiral amino acids using reversed-phase chromatography. The amino acids were separated by isocratic or gradient elution on a Mightysil RP-18 GP column with a mobile phase containing H<sub>2</sub>O, methanol, and 0.1% (v/v) formic acid. The enantiomers of the amino acids were fully separated with high resolution (<i>Rs</i> = 1.20–5.30) and high sensitivity (limit of detection: 85–4546 fmol) using PPZ-Pro-NHS derivatization and LC–MS analysis with both isocratic and gradient elution. The enantiomers of 16 amino acid mixtures were simultaneously separated in a single chromatographic run using a gradient mobile phase system. Thus, PPz-Pro-NHS can be used for chiral amine screening and authentication.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 4","pages":"718 - 730"},"PeriodicalIF":1.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949460","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":"Improvement of the Selectivity and Sensitivity of Analysis of Tetracycline Antibiotics Based on the ESI-MS Method with a Single-Quadrupole Mass Analyzer","authors":"A. V. Streletskiy, N. S. Antropova","doi":"10.1134/S1061934825700091","DOIUrl":"10.1134/S1061934825700091","url":null,"abstract":"<p>The article describes methodological approaches that can be used to improve the performance characteristics of a single-quadrupole mass analyzer for studying the residual content of small organic substances in an aqueous medium using tetracycline antibiotics as an example. To improve the selectivity of the analysis, it is proposed to use optimal parameters of electron optics in the source (voltage across the fragmentor) in order to achieve a high yield of product ions. It is shown that the sensitivity of the analysis can be improved by summing the signals of all the formed product ions.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 4","pages":"666 - 674"},"PeriodicalIF":1.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949485","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}
A. V. Pirogov, E. S. Chichkanova, A. S. Popov, V. V. Levkina, T. A. Bolotnik, M. V. Popik, A. A. Stepashkin, E. N. Grunina, O. M. Zolotilova
{"title":"Determination of Volatile Compounds from Lavender Flowers Using Passive Sorption on Novel Monolithic Butadiene-Nitrile Rubber and Silicon Carbide Materials by Thermal Desorption Gas Chromatography–Mass Spectrometry","authors":"A. V. Pirogov, E. S. Chichkanova, A. S. Popov, V. V. Levkina, T. A. Bolotnik, M. V. Popik, A. A. Stepashkin, E. N. Grunina, O. M. Zolotilova","doi":"10.1134/S1061934825700133","DOIUrl":"10.1134/S1061934825700133","url":null,"abstract":"<p>A novel composite material based on butadiene-nitrile rubber and silicon carbide (<b>BNR-SiC</b>) was synthesized and used for the first time to determine volatile components of lavender flowers by passive sorption, followed by thermal desorption and gas chromatography−mass spectrometry (<b>GC−MS</b>) identification. This material was demonstrated to capture almost the full range of organic compounds, exhibiting similar sorption/desorption efficiency and better thermal stability compared to Tenax TA. The chromatograms of lavender constituents obtained by passive sorption on Tenax TA and BNR-SiC composite are quite similar. Classes of compounds identified on the chromatograms include mono- and sesquiterpenes, their oxygenated derivatives, terpene alcohols, aromatic hydrocarbons, heterocyclic compounds, phenols, glycerides, linalool, linalyl acetate, eucalyptol, caryophyllene, linalool oxides, 1,3-glyceryl diacetate, and fatty acids, totaling 60 compounds. The approach of passive sorption on a BNR-SiC sorbent followed by thermal desorption GC−MS fingerprint analysis can provide a rough estimation of the compositional diversity and proximity of multi-herbal samples containing various groups of volatile terpene compounds.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 4","pages":"707 - 717"},"PeriodicalIF":1.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949580","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}
Muhammad Asghar, Mohammad Yaqoob, Masood Ahmed Siddiqui, Amir Waseem
{"title":"Analytical Applications of Chemiluminescence in Flow-Injection Systems","authors":"Muhammad Asghar, Mohammad Yaqoob, Masood Ahmed Siddiqui, Amir Waseem","doi":"10.1134/S1061934825700017","DOIUrl":"10.1134/S1061934825700017","url":null,"abstract":"<p>Chemiluminescence (<b>CL</b>) detection, in combination with the flow injection (<b>FI</b>) technique, provides simple instrumentation approach characterized by rapid response time, low limits of detection, and reliable methodologies for examining a broad spectrum of analytes in diverse scientific domains of analytical chemistry. This review describes the chemiluminescent reactions involving CL reagents and certain oxidants, highlighting their recent analytical applications in the analysis of significant analytes present in environmental, pharmaceutical, biological, and food matrices using the FI technique. The literature review includes key analytical studies published from 2018 to mid-2024. The review concludes with insights and future perspectives in this area of research.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 4","pages":"565 - 590"},"PeriodicalIF":1.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949582","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}
N. O. Goncharov, V. V. Tolmacheva, A. O. Melekhin, M. A. Biryukova, V. V. Apyari, S. G. Dmitrienko
{"title":"Dispersive Magnetic Solid-Phase Extraction of Magnetic Hypercrosslinked Polystyrene with Carbon Dioxide for the Multicomponent Extraction of Residues of 55 Veterinary Drugs from River Waters Before Their Determination by HPLC–MS/MS","authors":"N. O. Goncharov, V. V. Tolmacheva, A. O. Melekhin, M. A. Biryukova, V. V. Apyari, S. G. Dmitrienko","doi":"10.1134/S1061934825700054","DOIUrl":"10.1134/S1061934825700054","url":null,"abstract":"<p>Magnetic effervescent tablets consisting of magnetic hypercrosslinked polystyrene, sodium bicarbonate, citric acid and EDTA are proposed for multicomponent isolation of residues of 55 veterinary drugs of various classes (sulfonamides and trimethoprim, amphenicols, nitroimidazoles, β-lactams, quinolones, macrolides, pleuromutilins and lincosamides) from river waters by magnetic solid-phase extraction prior to their HPLC–MS/MS determination. Due to the intensive release of carbon dioxide during tablet dissolution, this process was conducted without using stirring devices, and the magnetic properties of the sorbent ensures its separation without centrifugation and filtration; as a result, the sample preparation procedure (solid-phase extraction) took less than 3 min. The method ensures recoveries from 79 to 122% and good reproducibility (RSD ≤ 12%). Drugs were identified by the exact masses of analyte ions formed during polarity-switching electrospray ionization. The matrix effect for all drugs was below 20%. The determination was carried out using the matrix calibration method; the limits of detection and quantification are 0.012 and 0.04 μg/L for most sulfonamides, trimethoprim, amphenicols, nitroimidazoles, macrolides, pleuromutilins and lincosamides, and 0.06 and 0.2 μg/L for β-lactams and quinolones, respectively.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 4","pages":"623 - 633"},"PeriodicalIF":1.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949438","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":"Facile Synthesis of Yttrium-Doped Cadmium Sulfide Nanocrystals for the Simultaneous Electrochemical Sensing of Dopamine, Uric Acid, Xanthine, and Hypoxanthine","authors":"Vinay Gopalappa, Ashwini Gulaganahalli Ramadasaiah, Nagaraju Kottam, Shivaraj Yellappa","doi":"10.1134/S1061934825700182","DOIUrl":"10.1134/S1061934825700182","url":null,"abstract":"<p>Yttrium-doped cadmium sulfide (<b>Y-CdS</b>) nanocrystals were synthesized by a co-precipitation method. The electrochemical behavior of the modified electrode, Y-CdS/glassy carbon electrode, was explored by voltammetric and electrochemical impedance studies. The electrochemical performance of the modified electrode demonstrated a remarkable enhancement in peak current for the oxidation of dopamine and was also used for the simultaneous determination of dopamine, uric acid, xanthine, and hypoxanthine, which exhibit a linear response for all these biomolecules. The modified electrode also demonstrated long-term stability, good reproducibility and successfully applied to the determination of dopamine in real samples, enabling rapid detection in practical applications.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 4","pages":"756 - 771"},"PeriodicalIF":1.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949455","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}
Wan Nurdini Wan Mohd Hassim, Wooi Meng Yew, Mohamed Izzharif Abdul Halim, Hukil Sino, Loong Chuen Lee
{"title":"Exploring Inter-Sample Variability of Malaysian Gasoline Using Attenuated Total Reflectance-Fourier Transform Infrared Spectroscopy and Multivariate Exploratory Methods for Forensic Investigation","authors":"Wan Nurdini Wan Mohd Hassim, Wooi Meng Yew, Mohamed Izzharif Abdul Halim, Hukil Sino, Loong Chuen Lee","doi":"10.1134/S1061934824701934","DOIUrl":"10.1134/S1061934824701934","url":null,"abstract":"<p>Determination of the source origin of fuel plays a paramount role in forensic investigations. The most probable location for selling questioned fuel seized from a crime scene can be inferred by determining the brand and quality grade of the fuel. In other words, insights into inter- and intra-sample variations of gasoline sold within a country could potentially contribute to developing reliable procedures for identifying gasoline sources. The current work aims to explore inter-gasoline variation based on their infrared (<b>IR</b>) fingerprints using multivariate exploratory tools. A total of 48 samples representing four brands (i.e., BHP, PET, PNAS, and S) with two different research octane numbers (RON95 and RON97) were purchased from eight pump stations in Selangor, Malaysia, over three different periods. The organic components of gasoline samples were analyzed by attenuated total reflectance-Fourier transform infrared (<b>ATR-FTIR</b>) spectroscopy with minimal sample preparation. Multivariate exploratory tools, including principal component analysis and hierarchical clustering analysis, were applied to reveal variations by brand, RON grade, pump station, and sampling period. Results showed that IR fingerprints of gasoline varied by the four source origins. BHP gasoline emerged as the most discriminative sample, associated with lower inter-sampling period variation. On the other hand, PET and PNAS were highly similar, with PET showing pronounced inter-pump station variation. In particular, S gasoline was readily discriminated by sampling periods and pump stations. In conclusion, coupling ATR-FTIR spectroscopy with chemometric techniques is potentially useful for determining gasoline source origins.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 3","pages":"455 - 466"},"PeriodicalIF":1.0,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143913803","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}