M. F. Vokuev, A. Yu. Oprunenko, A. V. Frolova, T. M. Baygildiev, I. A. Rodin
{"title":"Detection of Melittin, a Characteristic Peptide of Bee Venom, in Semisolid Dosage Forms Using Liquid Chromatography–High-Resolution Mass Spectrometry","authors":"M. F. Vokuev, A. Yu. Oprunenko, A. V. Frolova, T. M. Baygildiev, I. A. Rodin","doi":"10.1134/S1061934825700789","DOIUrl":"10.1134/S1061934825700789","url":null,"abstract":"<p>Due to its pharmacological and biological activity, bee venom is used in the production of various drugs and pharmaceutical forms, including ointments and creams. Melittin is the main component of bee venom, and its presence in a drug preparation is characteristic of the presence of bee venom as a constituent. An approach to the detection of this characteristic peptide component of bee venom in semisolid dosage forms, which involves recovery and preconcentration using solid-phase extraction followed by liquid chromatography with mass spectrometric detection, was proposed. The specificity of the detection procedure was validated, and the limit of detection was 0.1 μg/g.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 :","pages":"1575 - 1581"},"PeriodicalIF":1.1,"publicationDate":"2025-09-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145122309","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}
Pham Thi Gam, O. A. Tertyshnikova, A. N. Zyablov, A. Yu. Vyborny, N. A. Litvinova
{"title":"Determination of Antibiotics in Wastewaters Using Amperometric Sensors","authors":"Pham Thi Gam, O. A. Tertyshnikova, A. N. Zyablov, A. Yu. Vyborny, N. A. Litvinova","doi":"10.1134/S1061934825700790","DOIUrl":"10.1134/S1061934825700790","url":null,"abstract":"<p>Sensors are developed for the amperometric determination of the antibiotics Cefur and Ceftr in aqueous solutions. The sensor electrodes were coated with a molecularly imprinted polymer (MIP). To assess the selectivity and molecular recognition ability of the sensors, the imprinting factor and selectivity coefficient were determined. The imprinting factor reached 5.3 for MIP-Cefur and 5.1 for MIP-Ceftr. The results demonstrated that the MIPs exhibited higher selectivity and recognition capability for Cefur and Ceftr compared to non-imprinted polymers. The antibiotics were quantified in aqueous solutions using the calibration curve method. The experimentally found concentration ranges for Cefur and Ceftr were from 1.0 × 10<sup>–5</sup> to 0.1 g/L. The limits of detection were 3.5 × 10<sup>–6</sup> g/L for Cefur and 6.6 × 10<sup>–6</sup> g/L for Ceftr. MIP-modified sensors were tested in the determination of antibiotics in wastewaters. The findings confirmed the applicability of amperometric sensors based on molecularly imprinted polymers to the determination of Cefuroxime sodium and Ceftriaxone sodium in both model and real aqueous solutions.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 :","pages":"1582 - 1587"},"PeriodicalIF":1.1,"publicationDate":"2025-09-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145122328","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. S. Gubin, K. S. Sypko, A. A. Kushnir, P. T. Sukhanov
{"title":"Determination of Endocrine Disruptors in Bottom Sediments by Gas Chromatography–Mass Spectrometry with Analyte Preconcentration by Liquid–Liquid and Magnetic Dispersive Solid-Phase Extraction","authors":"A. S. Gubin, K. S. Sypko, A. A. Kushnir, P. T. Sukhanov","doi":"10.1134/S1061934825700777","DOIUrl":"10.1134/S1061934825700777","url":null,"abstract":"<p>A method is proposed for the extraction and preconcentration of six of the most common endocrine disruptors (dimethyl, diethyl, dibutyl phthalates; bisphenol A; and octyl- and nonylphenols) from river bottom sediments. The analytes are extracted by two-stage preconcentration. At the first stage, the analytes are extracted from an aqueous solution with an ionic liquid, 1-hexyl-3-methylimidazolium hexafluorophosphate in the presence of a surfactant (sodium dodecyl sulfate). The volumes of the extractant and surfactant solution (12 vol %) are 200 μL and 0.5 mL, respectively. Extraction duration is 2 min. At the second stage, magnetic dispersive solid-phase extraction with magnetic coals of plant origin modified with reversed phases of <i>n</i>-octyltrimethoxysilane and <i>n</i>-octadecyltrimethoxysilane is used. The recovery of analytes by liquid–liquid extraction is 91–99% and by magnetic solid-phase dispersive extraction, 89–99%. It is found that, during solid-phase dispersive extraction, the best conditions for the extraction of disruptors are achieved at pH 5.2–7.0, sorption duration of 5 min using a centrifuge (4000 rpm), and sorbent portion of 25 mg. The use of two-stage preconcentration in combination with gas chromatography–mass spectrometry ensures the determination of endocrine disruptors in bottom sediments at a level of 0.4–0.7 μg/kg.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 :","pages":"1561 - 1574"},"PeriodicalIF":1.1,"publicationDate":"2025-09-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145122412","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 Single Microfluidic Paper-Based Analytical Device for the Determination of Ammonia and pH Using Mulberry Fruit Extract as a Natural Indicator","authors":"Piyawan Phansi, Kodchakorn Inthichit, Mongkol Trongdee, Natcha Kaewkong, Duangjai Nacapricha","doi":"10.1134/S1061934825600854","DOIUrl":"10.1134/S1061934825600854","url":null,"abstract":"<p>This work presents a microfluidic paper-based analytical device (<b>µPAD</b>) designed for the screening and measurement of ammonia and pH, utilizing mulberry fruit extract as a natural indicator. For ammonia determination, the method is based on a membraneless gas-separation microfluidic device. The µPAD co-nsists of three layers: the upper layer serves as the detection area, featuring two circles with a diameter of 8 mm, where mulberry fruit extract at pH 3.07 and pH 4.93 is applied for the measurement of ammonia and pH, respectively. Ammonia gas is generated in the lower donor layer and diffuses through the gap in the middle layer to the acceptor layer. The concentration of ammonia is determined by analyzing the color change of the mulberry fruit extract indicator. Images of the colored detection zones are captured using a smartphone camera, and their color intensity is analyzed with ImageJ software. For pH measurement, the color change is compared to a standard pH scale ranging from 1 to 14. The proposed method offers a linear calibration range from 0 to 150 mg/L N, with a limit of detection of 4.89 mg/L N. The relative standard deviation was 3.43% (at 50 mg/L N, <i>n</i> = 10). This method was successfully applied to measure ammonia and pH in natural water, pond water, wastewater, and fertilizer samples, with recovery rates ranging from 95 to 109%. The results obtained from the µPAD correlated well with those from the spectrophotometric method for ammonia and a pH meter for pH values.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 8","pages":"1411 - 1421"},"PeriodicalIF":1.1,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144868791","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 Iodine in CsGeI3 by Inductively Coupled Plasma Atomic Emission Spectrometry","authors":"Sun Haifeng, Li Tian, Xu Qing, Zhang Lijiu","doi":"10.1134/S1061934825700698","DOIUrl":"10.1134/S1061934825700698","url":null,"abstract":"<p>An inductively coupled plasma atomic emission spectrometry (<b>ICP–AES</b>) method for the determination of iodine in CsGeI<sub>3</sub> perovskite materials has been developed. The method involves microwave digestion with a hydrochloric-nitric acid system (3 : 1) at 120°C for 10 min, followed by analysis using optimized ICP–AES parameters (radio frequency power: 1150 W, cooling gas flow: 12.5 L/min). The linear range of iodine determination was 1.00–60.00% with a determination coefficient (<i>R</i><sup>2</sup> = 0.999). Recovery rates ranged from 98.6 to 102.1%, and the relative standard deviation (<i>n</i> = 11) was ≤3.4%. The method demonstrated high accuracy and precision, validated through analysis of CsGeI<sub>3</sub> samples from diverse sources.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 8","pages":"1454 - 1460"},"PeriodicalIF":1.1,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144869040","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":"Indirect Spectrophotometric Method for the Determination of Dimethoate and Oxydemeton-Methyl Insecticides in Environmental Samples","authors":"Nisha Sharma, Srishti Shekhar","doi":"10.1134/S1061934825700686","DOIUrl":"10.1134/S1061934825700686","url":null,"abstract":"<p>Insecticides like dimethoate and oxydemeton-methyl are essential for crop protection, supporting food production. However, their overuse raises environmental and food safety concerns due to contamination and residues. A new spectrophotometric method was developed to monitor these insecticides in formulations and environmental samples such as water, grains, and vegetables. The proposed method is based on the redox reaction of the thiol (the hydrolytic product formed in an alkaline medium) in both insecticides, with ferric chloride, leading to the formation of Fe<sup>2+</sup>, which subsequently reacts with 1,10<b>-</b>phenanthroline to form colored complexes, measurable at 510 nm. The method obeys Beer’s law within the concentration ranges of 0.46–13.74 µg/mL for dimethoate and 0.49–14.76 µg/mL for oxydemeton-methyl. Reaction parameters such as hydrolysis time, solvent type, heating time, and reagent concentration were optimized to enhance the sensitivity and stability of the method. The recovery results from water and environmental samples demonstrated the good accuracy and precision of the method, with recoveries of 89–100.8% for dimethoate and 89.9–99% for oxydemeton-methyl, and a relative standard deviation of 0.29–1.96 and 0.23–1.91% for dimethoate and oxydemeton-methyl, respectively.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 8","pages":"1434 - 1444"},"PeriodicalIF":1.1,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144868793","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}
Mohammad Reza Jamali, Saeed Khaleghi-Gorji, Reyhaneh Rahnama
{"title":"Assessment of In Situ Sorbent Formation Solid-Phase Extraction for the Determination of Cadmium in Natural Water Samples and Plant Leaves by Flame Atomic Absorption Spectrometry","authors":"Mohammad Reza Jamali, Saeed Khaleghi-Gorji, Reyhaneh Rahnama","doi":"10.1134/S1061934825601136","DOIUrl":"10.1134/S1061934825601136","url":null,"abstract":"<p>A novel solid-phase extraction procedure was developed for the preconcentration and measurement of cadmium in plant leaves (lettuce and tobacco) and water samples utilizing flame atomic absorption spectrometry. This proposed method involves the in situ formation of an insoluble ion-pairing salt to be used as a sorbent. Cetyltrimethylammonium bromide was utilized as a cationic surfactant, and perchlorate was added as an ion-pairing agent. Cadmium(II) ions were selectively extracted after forming a complex with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol. The variables were optimized, and method validation was performed. The limit of detection and limit of quantification were, respectively, 0.31 and 1.1 μg/L. With a preconcentration factor of 40 and a relative standard deviation of 2.6%, the method demonstrates promise for detecting low levels of cadmium. The monitoring of cadmium in real samples was successfully carried out using the suggested approach.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 8","pages":"1445 - 1453"},"PeriodicalIF":1.1,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144868794","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":"Applications of Smart Materials in Sample Preparation for Biological and Environmental Analysis","authors":"D. A. Karpitskiy, L. A. Kartsova","doi":"10.1134/S1061934825700595","DOIUrl":"10.1134/S1061934825700595","url":null,"abstract":"<p>Sample preparation of naturally occurring matrices necessitates the development of highly sensitive and selective methods for the extraction and preconcentration of biologically active compounds. Smart materials are highly promising in this area and are selected for solving for specific analytical tasks. This review examines the main categories of such materials, including ionic liquids, eutectic solvents, nanomaterials, metal-organic frameworks, covalent organic frameworks, and molecularly imprinted polymers. It highlights their unique properties and provides specific examples of their application to chemical analysis between 2020 and 2025. The article discusses the use of smart materials in the analysis of biological fluids and environmental samples, available microextraction techniques, and subsequent quantification methods. It emphasizes the advancements achieved in comparison to the previously established approaches.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 8","pages":"1313 - 1330"},"PeriodicalIF":1.1,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144869111","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}
Z. A. Temerdashev, P. G. Abakumov, A. G. Abakumov, M. A. Bol’shov
{"title":"Microextraction Separation and Determination of Inorganic Arsenic Species by Inductively Coupled Plasma Mass Spectrometry in Natural Waters","authors":"Z. A. Temerdashev, P. G. Abakumov, A. G. Abakumov, M. A. Bol’shov","doi":"10.1134/S1061934825700613","DOIUrl":"10.1134/S1061934825700613","url":null,"abstract":"<p>The results of microextraction separation and ICP–MS determination of inorganic arsenic species in natural waters are presented. The necessity of the separate quantification of analytes is justified, as arsenites exhibit toxicity dozens of times higher than arsenates. Separation was performed by the selective liquid–liquid microextraction of As(III) complexes with sodium diethyldithiocarbamate into an organic phase. Extraction conditions were optimized to achieve the highest recovery of As(III) complexes at approximately 95%. The As(III) complexes with sodium diethyldithiocarbamate were extracted into the organic phase using carbon tetrachloride as an extractant and methanol as a dispersant. Matrix effects of elements on analyte extraction from water were eliminated by performing a double microextraction of the analytes. Total inorganic arsenic and As(V) concentrations were determined by an ICP–MS analysis of the original water samples and their aqueous extracts obtained after the separation of inorganic arsenic species. The concentration of As(III) in water was calculated as the difference between total arsenic and As(V) concentrations. The limits of detection for As(III) and As(V) in water were equal, at 0.010 μg/L, within a linearity range of 0.05 to 100 μg/L, <i>R</i><sup>2</sup> = 0.9998. The accuracy of the determination of inorganic arsenic species in water was confirmed by the standard addition method. The analytical procedure was validated using model waters and real samples of drinking and natural waters.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 8","pages":"1345 - 1353"},"PeriodicalIF":1.1,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144868741","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}
Luna Maslov Bandić, Kristina Vlahoviček-Kahlina, Slaven Jurić, Marija Sigurnjak Bureš
{"title":"Quantification of Phenolic Compounds in Different Tissues and Juice of Satsuma Mandarin Fruit by High-Performance Liquid Chromatography","authors":"Luna Maslov Bandić, Kristina Vlahoviček-Kahlina, Slaven Jurić, Marija Sigurnjak Bureš","doi":"10.1134/S1061934825600623","DOIUrl":"10.1134/S1061934825600623","url":null,"abstract":"<p>This study investigates the distribution and quantification of phenolic compounds in different tissues (juice, pulp, and peel) of six Satsuma mandarin (<i>Citrus unshiu</i>) varieties cultivated in Croatia. Narirutin and hesperidin were the dominant flavonoids in mandarin juice and pulp, with the highest concentrations observed in the “Okitsu” variety. Peel samples exhibited a higher flavonoid content, particularly hesperidin and polymethoxylated flavones, such as nobiletin and tangeretin. Extractable and bound phenolic acids, including ferulic, caffeic, and <i>p</i>-coumaric acids, were quantified. The “Okitsu” variety showed the highest levels of most phenolic acids. The optimized high-performance liquid chromatography method demonstrated high precision and sensitivity, enabling efficient quantification of 18 phenolic compounds. This study provides valuable insights into the phenolic composition of Satsuma mandarins, contributing to citrus quality assessment, dietary applications, and sustainable utilization of citrus waste.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 8","pages":"1461 - 1470"},"PeriodicalIF":1.1,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144869125","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}