Z. A. Temerdashev, T. K. Chubukina, N. V. Kiseleva
{"title":"Determination of Volatile Components in Various Extracts of Wild Chamomile (Matricaria chamomilla L.) Flowers by Gas Chromatography–Mass Spectrometry","authors":"Z. A. Temerdashev, T. K. Chubukina, N. V. Kiseleva","doi":"10.1134/S1061934824701971","DOIUrl":"10.1134/S1061934824701971","url":null,"abstract":"<p>The work is devoted to the assessment of the efficiency of the extraction of volatile organic compounds from wild chamomile (<i>Matricaria chamomilla</i> L.) flowers. Volatile organic compounds (<b>VOCs</b>) in extracts of flowers of wild chamomile obtained by Ginsberg hydrodistillation, liquid–liquid extraction, and dispersive liquid–liquid microextraction and also by subcritical and ultrasound-assisted (US) extraction were determined by gas chromatography–mass spectrometry. Volatile compounds were identified by comparing the recorded mass spectra of components with the data of NIST07 and WILEY8 databases. Analyte concentrations in the extracts were estimated by the internal normalization of peak areas and by the internal standard method with thujone in acetone. The concentrations of VOCs were determined in the essential oil and aromatic water obtained by Ginsberg hydrodistillation, under subcritical conditions, and upon US treatment of acetone extracts from wild chamomile flowers. β-Farnesene, α-bisabolol oxide B, and bisabolol oxide A were identified as macrocomponents of essential oil. α-Bisabolol oxide B, α-Limonene diepoxide, and bisabolol oxide A were identified as macrocomponents of a hexane extract from aromatic water. The main component of acetone extracts from wild chamomile flowers under subcritical conditions and upon US treatment was en-in-dicycloether. It was shown that the concentration of VOCs in the wild chamomile aromatic water is higher than that in the essential oil and the list of compounds is wider.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 3","pages":"501 - 514"},"PeriodicalIF":1.0,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143913809","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":"High-Throughput Determination of Trace-Level Peroxides in Reagents and Packaging Materials Based on a Simple 96-Well Plate Ultraviolet Spectrometric Method","authors":"Danyi Yang, Jingwei Lan, Jiao Chen, Yuyu Wu, Wen Qian, Jiangbin Han","doi":"10.1134/S1061934824701922","DOIUrl":"10.1134/S1061934824701922","url":null,"abstract":"<p>The aim of the present study was to develop a sensitive, high-throughput 96-well plate ultraviolet spectrometric method for the determination of peroxide value at trace levels in reagents and packaging materials. The analysis was carried out under acid-free conditions to minimize or prevent reactions between iodine molecules and oxygen in the air, thereby ensuring the accuracy and repeatability of the experiments. The wavelength was set at 360 nm. The analytical procedure was validated by evaluating linearity (<i>r</i><sup>2</sup> = 0.9998), precision (intra- and inter-day precision were less than 0.90 and 6.20%, respectively.), accuracy (100–110% of the spiked amount), and limits of detection (<b>LOD</b>) and quantification (<b>LOQ</b>). The LOD and LOQ were confirmed to be 20 and 50 ng/mL, respectively. This high-throughput technique reduces the risk of chemical changes during analysis due to time inconsistencies, which benefits the accuracy and reproducibility of results. The proposed method was then successfully applied to determine trace amounts of peroxides in ethyl acetate and packaging material samples. Overall, the present study offers an accurate and sensitive method for measuring trace-level peroxides.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 3","pages":"448 - 454"},"PeriodicalIF":1.0,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143913804","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}
Sara Abdel Basset Galal, Eman Saad Elzanfaly, Emad Mohamed Hussien, Enas Abdel Hakim Amer, Hala Elsayed Zaazaa
{"title":"Sustainable Thin-Layer Chromatographic Method for the Determination of Ipriflavone and Vitamins in Bone Health Supplements","authors":"Sara Abdel Basset Galal, Eman Saad Elzanfaly, Emad Mohamed Hussien, Enas Abdel Hakim Amer, Hala Elsayed Zaazaa","doi":"10.1134/S1061934824701958","DOIUrl":"10.1134/S1061934824701958","url":null,"abstract":"<p>A simple, high-performance thin-layer chromatographic method was developed to separate and quantify ipriflavone, ascorbic acid, pyridoxine, and vitamin D<sub>3</sub> in bulk and combined pharmaceutical formulations. Elution was achieved using a developing system consisting of toluene, dichloromethane, methanol, and glacial acetic acid (5 : 3 : 3 : 0.2, v/v) on an F<sub>254</sub> silica gel stationary phase, followed by densitometric measurement of the separated bands at 254 nm. Validation of the proposed method was performed according to the ICH guideline Q2(R1). The method was validated in the concentration ranges of 2–12, 4–22, 0.4–2.2, and 0.15–1.35 µg/band for ascorbic acid, pyridoxine, ipriflavone, and vitamin D<sub>3</sub>, respectively. The method can be used for the selective analysis of the stated compounds in both bulk and combined pharmaceutical formulations. The developed method was eco-evaluated using two assessment tools, namely the Green Analytical Procedure Index and the Analytical GREEnness metric, confirming the method’ s eco-friendliness. The whiteness of the proposed method was evaluated and compared to that of a published high-performance liquid chromatography method for separating the same mixture. The thin-layer chromatography method showed a better whiteness profile and was deemed suitable for routine quality control analysis.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 3","pages":"480 - 489"},"PeriodicalIF":1.0,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143913855","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}
M. S. Ermolin, A. I. Ivaneev, E. Yu. Savonina, R. Kh. Dzhenloda
{"title":"Extraction of Microplastics from River Water in a Rotating Coiled Column Using a Water–Oil System","authors":"M. S. Ermolin, A. I. Ivaneev, E. Yu. Savonina, R. Kh. Dzhenloda","doi":"10.1134/S1061934824701909","DOIUrl":"10.1134/S1061934824701909","url":null,"abstract":"<p>Determination of the microplastics content of natural waters is an important task in assessing the degree of water body pollution, identifying pollution sources, and evaluating potential risks for aquatic ecosystem inhabitants and water consumers. Solving this problem primarily falls within the realm of analytical chemistry, with separation methods for particles playing a crucial role. This work for the first time presents a potential application of the method of continuous-flow microplastic separation in a rotating coiled column using a water–oil system for assessing the microplastics content in river water. Microplastics in the extracted particle samples were determined by pyrolytic gas chromatography with mass spectrometric detection (pyro-GC–MS). A water sample from the Moskva River was analyzed. Using a water–castor oil system, 1.8 mg/L of suspended particles were extracted from the river water. A procedure for the digestion of the organic matter of the sample (30% H<sub>2</sub>O<sub>2</sub>) reduced the mass of the extracted particles to 0.4 mg/L. The residual fraction was analyzed by optical microscopy. According to the pyro-GC–MS data, the total microplastics content in the test water sample was 109 µg/L, accounting for 1.4% of the total suspended particle content of the sample. Five types of microplastics were identified: polyethylene, polypropylene, acrylonitrile butadiene styrene, acryl–butadiene rubber, and polyethylene terephthalate, with polyethylene being the predominant type (97 µg/L). The proposed method offers promise for assessing the microplastics content in natural waters.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 3","pages":"432 - 441"},"PeriodicalIF":1.0,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143913805","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":"Application of Smartphones to Measurements of Reducing Power Related to Antioxidant Activity","authors":"Si Eon Lee, Chang Soon Huh","doi":"10.1134/S1061934824701910","DOIUrl":"10.1134/S1061934824701910","url":null,"abstract":"<p>Antioxidants effectively prevent oxidation by forming non-toxic products, making them of interest to food scientists, health professionals, and the public. Vitamin C, recognized for its antioxidant properties, has traditionally been evaluated for its reducing power using UV-Vis spectrophotometry and smartphone applications, though the latter has faced methodological limitations. This study aimed to improve and validate smartphone-based methods for assessing the antioxidant activity of beverages using ferric reducing antioxidant power analysis. The results showed a strong correlation between the reducing power of vitamin C measured by UV-Vis spectrophotometry (<i>R</i><sup>2</sup> = 0.9913) and smartphone applications (<i>R</i><sup>2</sup> = 0.9823), suggesting that the developed smartphone method is a viable and effective tool for identifying the antioxidant properties of commercially available beverages.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 3","pages":"442 - 447"},"PeriodicalIF":1.0,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143913807","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 Biologically Active Components of Rhodiola rosea in Extracts of Plant Raw Materials by HILIC–MS/MS","authors":"S. A. Nuikin, Yu. V. Timchenko, I. A. Rodin","doi":"10.1134/S1061934824701740","DOIUrl":"10.1134/S1061934824701740","url":null,"abstract":"<p>A simple, rapid, and highly sensitive method for the simultaneous determination of the main components of <i>Rhodiola rosea</i> (rosin, salidroside, rosarin, and rosavin) in a wide concentration range by hydrophilic chromatography–tandem mass spectrometry is developed. The conditions for the extraction (extractant type and composition, extraction time) of the main components from <i>Rhodiola rosea</i> root samples, chromatographic separation and detection of these compounds are selected, and the performance characteristics of the proposed approach are evaluated. The limits of detection are 250, 2.4, 2.3, and 5.4 ng/mL, and the linearity ranges are 1–100, 0.01–10, 0.01–10, and 0.01–100 μg/mL for rosin, salidroside, rosarin and rosavin, respectively. The developed approach is tested in an analysis of real samples of the pharmaceutical product and of plant raw material.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 2","pages":"267 - 278"},"PeriodicalIF":1.0,"publicationDate":"2025-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143861267","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. T. Afandiyeva, A. M. Maharramov, F. M. Chiragov
{"title":"Equilibrium and Kinetic Studies of Silver(I) Preconcentration on Synthetic Sorbents","authors":"N. T. Afandiyeva, A. M. Maharramov, F. M. Chiragov","doi":"10.1134/S1061934824701776","DOIUrl":"10.1134/S1061934824701776","url":null,"abstract":"<p>A new synthetic sorbent (<b>S</b><sub><b>1</b></sub>) was obtained based on a copolymer of styrene with maleic anhydride and norsulfazole (<b>S</b>) with subsequent modification by the reagent 4,4'-(ethane-1,2-diylbis(azanylidene))bis(pentan-2-one). The structure of the sorbent <b>S</b> was studied by IR and UV spectrometry. The sorption of Ag(I) ions on the sorbents S and S<sub>1</sub> was studied. The influence of various parameters on the sorption process was studied, i.e., pH, contact time, and initial concentration of the metal ion. The results of the conducted studies were presented by various models of adsorption isotherms and kinetic models. According to the results of the studies, sorption is best characterized by the Langmuir model and the pseudo-second-order kinetic model. The maximum static sorption capacity was 420.08 mg/g for sorbent S and 577.24 mg/g for sorbent S<sub>1</sub>. For adsorption studies, a solution of Ag(I) of a concentration of 2 × 10<sup>–3</sup> M was used in the work. Static sorption studies were carried out at room temperature. At the final stage, the process of the desorption of the absorbed silver ions was carried out. For this purpose, mineral (HNO<sub>3</sub>) and organic (CH<sub>3</sub>COOH) acids were used in the concentration range 0.5–2.0 M. Synthetic sorbents S and S<sub>1</sub> were used to extract silver(I) from mushrooms. The results have shown that the modification of the chelating adsorbent with the reagent 4,4'-(ethane-1,2-diylbis(azanylidene))bis(pentan-2-one) was accompanied by an increase in the sorption capacity, i.e., a simultaneous increase in the efficiency of Ag(I) ion extraction by the obtained synthetic sorption material. Comparative characteristics of the maximum adsorption capacities <i>q</i><sub>max</sub> of various adsorbents with respect to Ag(I) showed that the adsorbents S and S<sub>1</sub> have higher sorption capacity.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 2","pages":"299 - 308"},"PeriodicalIF":1.0,"publicationDate":"2025-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143861270","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":"An Approach to Optimizing Parameters of Mass Spectrometric Detection in the Identification of Trace Amounts of Highly Toxic Substances","authors":"M. Sh. Aigumov, S. A. Savchuk","doi":"10.1134/S1061934824701703","DOIUrl":"10.1134/S1061934824701703","url":null,"abstract":"<p>This study describes a procedure for optimizing the following parameters: scanning rate, the duration of selective transition registration (dwell time), and the delay between transitions from one selective transition to another (pause time). The study employed a liquid chromatograph coupled with a triple quadrupole mass spectrometric detector (LC–MS/MS Shimadzu 8050). Chromatographic separation was carried out on a Phenomenex Kinetex C18 reversed-phase column. Mobile phase A consisted of a 0.1% solution of formic acid in water with an addition of 10 mmol/L ammonium formate. Mobile phase B consisted of a 0.1% solution of formic acid in methanol with an addition of 10 mmol/L ammonium formate. The optimal parameters for confirmatory methods were determined: the dwell time of the selective transition was at least 10 ms, the pause time between the transitions was 1 ms, and the scanning rate ranged from 1000 to 5000 scans per second. This procedure was successfully applied to routine chemical-toxicological studies of urine samples with low concentrations of various narcotic and pharmaceutical substances.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 2","pages":"232 - 241"},"PeriodicalIF":1.0,"publicationDate":"2025-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143861117","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":"An Efficient Reversed-Phase High-Performance Liquid Chromatography-Based Approach for the Determination of Methotrexate in Biological Fluids","authors":"Mohsin Ali, Saeed Ahmed Lakho, Nurgali Akylbekov, Dovzhenko Alexey, Rustem Zairov","doi":"10.1134/S1061934824701831","DOIUrl":"10.1134/S1061934824701831","url":null,"abstract":"<p>In this work, a reversed-phase high-performance liquid chromatography method is reported for the determination of methotrexate (<b>MTX</b>), an anticancer drug. The method was found to be simple, sensitive, accurate, and precise. It was validated for the determination of the drug in human serum samples. For this purpose, spiking of the drug and internal standard (<b>IS</b>) was performed in drug-free plasma to assess the method’s applicability. p-Aminoacetophenone was employed as an IS. Protein precipitation was carried out using 2 M trichloroacetic acid, followed by centrifugation. MTX and IS were isolated using a C18 analytical column. The interference of the method was evaluated using blank plasma from six different subjects, and no interference was observed. The method demonstrated a linear response in the range of 300–20 000 ng/mL, with limits of detection and quantification of 1.82 and 6.07 ng/mL, respectively. The method was validated according to FDA and ICH guidelines Q2(R2), with intra- and inter-day accuracy and precision values within allowable limits. Using this method, ≥50% recovery of the drug was achieved from human blood plasma.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 2","pages":"358 - 363"},"PeriodicalIF":1.0,"publicationDate":"2025-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143861142","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}
I. V. Nikolaev, A. M. Bajkova, E. H. Galeeva, A. M. Grigoryev
{"title":"Detection of Metabolites of the New Synthetic Cannabinoid MDMB-4en-PINACA in Human Urine by Liquid and Gas Chromatography–Mass Spectrometry","authors":"I. V. Nikolaev, A. M. Bajkova, E. H. Galeeva, A. M. Grigoryev","doi":"10.1134/S1061934824701752","DOIUrl":"10.1134/S1061934824701752","url":null,"abstract":"<p>MDMB-4en-PINACA is a new synthetic psychoactive compound that has been widely distributed in Russia since at least 2020 and has high activity against the human cannabinoid receptor CB1. Its distinctive feature is the presence of an <i>N</i>-pentene residue, which is rare for this group of compounds. The significant hydrophobicity of MDMB-4en-PINACA, like most other synthetic cannabimimetics distributed on the world markets, causes almost complete biotransformation of the original compound and its extremely low content in urine. Hence, it follows that its metabolites should be identified, the detection of which would indicate the use of MDMB-4en-PINACA. To solve this problem, gas and liquid chromatography–mass spectrometry analysis was used, including high-performance chromatography–mass spectrometry with a quadrupole time-of-flight detector and a three-dimensional ion trap detector equipped with an electrospray ionization source. A number of putative metabolites of MDMB-4en-PINACA were detected in human urine, which were identified as products of hydrolysis, mono- and dihydroxylation, reduction, dihydrodiol formation, carboxylation, carboxylation with elimination of the methylene group, <i>N</i>-dealkylation, and combinations of these processes. A number of metabolites were found in the form of glucuronides. The results obtained are in good agreement with published data. The search for the products of hydrolysis, dihydroxylation, and dihydrodiol formation is optimal for routine chemical toxicological and forensic chemical analysis of urine by gas chromatography-mass spectrometry, while it is also recommended to detect glucuronides of hydrolysis products and dihydrodiol formation with the use of liquid chromatography–mass spectrometry.</p>","PeriodicalId":606,"journal":{"name":"Journal of Analytical Chemistry","volume":"80 2","pages":"279 - 292"},"PeriodicalIF":1.0,"publicationDate":"2025-04-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143861268","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}