Gabriela Lemos Ribeiro de Souza , Amanda de Paula Oliveira , Paulo Salles Neto , Jhonatan Bispo de Oliveira , Cassiano Lino dos Santos Costa , Patterson Patricio de Souza , Marina Bicalho Silveira , Ildefonso Binatti
{"title":"Strategies for the development and optimization of green acetonitrile-free HPLC methods for application in pharmaceutical analysis","authors":"Gabriela Lemos Ribeiro de Souza , Amanda de Paula Oliveira , Paulo Salles Neto , Jhonatan Bispo de Oliveira , Cassiano Lino dos Santos Costa , Patterson Patricio de Souza , Marina Bicalho Silveira , Ildefonso Binatti","doi":"10.1016/j.microc.2025.113659","DOIUrl":"10.1016/j.microc.2025.113659","url":null,"abstract":"<div><div>In the pharmaceutical industry, high-performance liquid chromatography (HPLC) is of central importance for quality control and the analysis of active pharmaceutical ingredients. Conventional HPLC methods commonly use acetonitrile (ACN) due to its favorable properties, but it’s expensive, toxic, and causes environmental damage, making it necessary to look for safer alternatives. This study presents a systematic approach to developing and optimizing an HPLC pharmaceutical analysis method by replacing ACN and phosphate buffer with methanol and trifluoroacetic acid (TFA). The method was validated for the purity analysis of the radiopharmaceutical PSMA-1007 (<sup>18</sup>F) and demonstrates a change towards more environmentally friendly methods in chromatographic analysis. Using multivariate experimental designs, the method was optimized to achieve efficient separation with methanol and TFA. The new method showed comparable performance to conventional methods, is cheaper, and offers environmental benefits such as lower solvent toxicity and lower ecological impact. This work emphasizes the importance of integrating green chemistry principles into method development and provides a guide for applying these practices to various pharmaceutical analyses.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"213 ","pages":"Article 113659"},"PeriodicalIF":4.9,"publicationDate":"2025-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143844804","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Qingwei Zhou , Meiqing Jin , Li Fu , Cheng-Te Lin , Weihong Wu
{"title":"From separation to identification: Microplastic detection and analyses in soils","authors":"Qingwei Zhou , Meiqing Jin , Li Fu , Cheng-Te Lin , Weihong Wu","doi":"10.1016/j.microc.2025.113652","DOIUrl":"10.1016/j.microc.2025.113652","url":null,"abstract":"<div><div>Microplastics (MPs) detection in soil environments presents unique analytical challenges due to matrix complexity and diverse particle characteristics. This review comprehensively examines current technologies and methodological approaches for detecting and characterizing MPs in soil matrices. Sample preparation techniques, including physical pretreatment, chemical digestion, and various separation methods such as density-based, electrostatic, oil-based, and magnetic separation, are critically evaluated. The review highlights how different analytical methods, from traditional microscopy to advanced spectroscopic techniques, complement each other in MP identification and quantification. Recent developments in artificial intelligence and deep learning applications for automated MP analysis are also discussed. The distribution patterns of MPs across different soil environments reveal significant variations, with agricultural soils showing concentrations ranging from 420–1290 particles/kg, urban soils containing 1750–12,200 particles/kg, and specialized ecosystems exhibiting unique MP profiles. Regional hotspots of MP contamination are identified, particularly in areas with intensive agricultural practices and inadequate waste management. The review emphasizes how both anthropogenic activities and natural factors influence MP abundance and characteristics in soils, with polymer types predominantly consisting of polyethylene, polypropylene, and polyvinyl chloride. This comprehensive analysis provides insights into current methodological advances while highlighting areas requiring further research and standardization in soil MP analysis.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"213 ","pages":"Article 113652"},"PeriodicalIF":4.9,"publicationDate":"2025-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143839389","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Development of ultrasonic assisted extraction and salting out liquid-liquid extraction techniques for agricultural environmental monitoring of pyroxasulfone and dietary risk assessment","authors":"Pervinder Kaur , Harshdeep Kaur , Harmeet Kaur , Tarundeep Kaur","doi":"10.1016/j.microc.2025.113662","DOIUrl":"10.1016/j.microc.2025.113662","url":null,"abstract":"<div><div>The optimization of extraction methods for monitoring herbicide residues is crucial for ensuring food safety and environmental sustainability. The present study focuses on optimizing ultrasound-assisted extraction (UAE) and salting out liquid-liquid extraction (SALLE) techniques for the efficient extraction of pyroxasulfone from soil, wheat and water. Various factors such as solvent type and volume, ultrasonication time and temperature, extraction cycle, sample-to-solvent ratio, salt type and its concentration were optimized to achieve the highest extraction efficiency. A mathematical model was constructed using the Box-Behnken design to represent the relationship between the variables and the response (percent recovery). The developed method demonstrated high accuracy and precision for determining pyroxasulfone in soil, wheat and water with mean percent recoveries ranging from 81.6 to 100.2 % and relative standard deviation < 10 %. Degradation studies revealed that at the time of harvest, pyroxasulfone residues in both soil and wheat grain were below detectable limits (<0.01 µg g<sup>−1</sup>), indicating effective degradation and minimal risk of residual contamination. HQ for pyroxasulfone was 0.113 indicating that there is no dietary risk associated with the consumption of rice containing pyroxasulfone residues. Additionally, environmental sustainability assessments using AGREE and GAPI metrics indicated the methods are green, offering low environmental impact and high efficiency. These findings underline the practical applicability of optimized UAE and SALLE techniques for pyroxasulfone residue analysis in agricultural environments, emphasizing their potential for routine monitoring and compliance with food safety standards.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"213 ","pages":"Article 113662"},"PeriodicalIF":4.9,"publicationDate":"2025-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143847773","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yingying Du , Qing Liu , Yong Zhao , Gangbing Zhu , Zongmian Zhang , Yinhui Yi
{"title":"Homogeneous electrochemical and colorimetric dual-model analysis of tetracycline based on target-stimulated peroxidase like activity of MIL(Fe3Ni)-88B","authors":"Yingying Du , Qing Liu , Yong Zhao , Gangbing Zhu , Zongmian Zhang , Yinhui Yi","doi":"10.1016/j.microc.2025.113651","DOIUrl":"10.1016/j.microc.2025.113651","url":null,"abstract":"<div><div>Tetracycline (TC) is an effective antibiotic that is extensively used. However, incomplete use of TC would leave residues in various environmental substrates, and excessive accumulation of TC can cause permanent damage to organisms and human health. Consequently, it is crucial to develop a fast and simple TC detection technique. In this work, a hydrothermal approach was used to create an amino functionalized bimetallic organic framework of iron and nickel (MIL(Fe<sub>3</sub>Ni)-88B) for homogeneous electrochemical (HEC) and colorimetric detection of TC. The synergistic effects of Ni and Fe enhance the redox capacity of MIL(Fe<sub>3</sub>Ni)-88B, and the amino group on its surface can bind with TC through a hydrogen-bonding interaction, which causes the electronic interactions and further enhance the peroxidase-like (POD-like) activity of MIL(Fe<sub>3</sub>Ni)-88B. Thus, with H<sub>2</sub>O<sub>2</sub> and o-phenylenediamine (OPD) as reaction substrate, the Fenton reaction is enhanced by the transfer of the electron between TC and MIL(Fe<sub>3</sub>Ni)-88B, enabling HEC detection of TC. Meanwhile, OPD could be oxidized to yellow 2,3-diaminophenylazine (DAP) under the catalysis reaction, providing feasibility for colorimetric detection of TC. The constructed dual-model analysis of TC achieves a wide linear range of 0.01 ∼ 10.0 μM for HEC detection and 0.25 ∼ 25.0 μM for colorimetric method, respectively, coupled with the low detection limits of 0.003 and 0.086 μM. Additionally, due to the unique structure of MIL(Fe<sub>3</sub>Ni)-88B, it can be used for highly effective detection of TC in water samples, and the detection of TC in real water samples based on the dual-model strategy has high recoveries between 97.04 % and 103.76 %.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"213 ","pages":"Article 113651"},"PeriodicalIF":4.9,"publicationDate":"2025-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143835155","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Jorge Lopez-Tellez , Israel S. Ibarra , Eva M. Santos , Alicia C. Mondragon-Portocarrero , Jose A. Rodriguez
{"title":"Aldehydes determination in edible oil samples employing 1-Naphthalenyl hydrazine as derivatizing agent followed by HPLC-FLD","authors":"Jorge Lopez-Tellez , Israel S. Ibarra , Eva M. Santos , Alicia C. Mondragon-Portocarrero , Jose A. Rodriguez","doi":"10.1016/j.microc.2025.113658","DOIUrl":"10.1016/j.microc.2025.113658","url":null,"abstract":"<div><div>Aldehydes formation in foods is the result of processing or degradation steps. These compounds provoke deterioration in taste, flavor, odor, color, texture and appearance, and nutritional value could be affected, and moreover potential adverse health effects could be derived. In this context, their analysis is essential in quality control. Therefore, this work proposes a fluorescent derivatization methodology based on 1-Naphthalenyl hydrazine as derivatizing agent for the pentanal, hexanal, heptanal, octanal, nonanal, and decanal determination followed by HPLC-FLD, obtaining limits of detections in the interval of 4.0–6.2 µg L<sup>−1</sup>. The derivatization process was optimized through full factorial and Box-Behnken experimental design and subsequently validated and applied to aldehyde determination in edible oil samples. The proposed derivatization methodology is efficient with adequate precision (expressed as relative standard deviation <10 %) and accuracy (92.57–109.68 %). The proposed derivatization method offers a competitive alternative to existing approaches that employ agents such as 2,4-dinitrophenylhydrazine, di(pyrrol-2-yl)methanone, or other derivatizing compounds. Moreover, the limits of detection obtained by fluorescence are comparable to those of chromatography systems accoupled to mass spectrometry. The methodology was applied to the quantification of the total long-chain aldehyde content, observing excellent perspectives in food quality control, so it could be applied to several aldehydes and complex samples.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"213 ","pages":"Article 113658"},"PeriodicalIF":4.9,"publicationDate":"2025-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143851624","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Chen Yang , Zhe Zhuang , Xiyu Zhang , Ziyi Ren , Danling Sun , Ping Wu , Jinzhou Liu , Wei Wu , Xuerong Chen
{"title":"Electroactive Fe-MOFs as an internal reference for ratiometric electrochemical sensing of 17β-estradiol with reinforcement of graphene nanosheets","authors":"Chen Yang , Zhe Zhuang , Xiyu Zhang , Ziyi Ren , Danling Sun , Ping Wu , Jinzhou Liu , Wei Wu , Xuerong Chen","doi":"10.1016/j.microc.2025.113650","DOIUrl":"10.1016/j.microc.2025.113650","url":null,"abstract":"<div><div>Ratiometric strategy is very effective to improve the reproducibility and reliability of electrochemcial sensors. Herein, a novel internal reference probe namely Fe-based MOFs (MIL-101), was adopted to provide the reference signal due to its obvious Fe oxidation behavior, without the necessary of literatural extensively used fixing electroactive small molecules. Besides, by introducing graphene nanosheet (GS), the resulting MIL-101/GS composite displayed remarkably reinforced electrochemcial active surface, electron transfer kinetics and adsorptive property. Compared to individual components, the composite demonstrated notably improved oxidation signals for both Fe and 17β-estradiol (E2) owing to the combined effects of MIL-101 and GS working together. Based on the dual-signal output model, a sensitive and reliable ratiometric electrochemcial sensor for E2 was readily constructed, possessing a broad linear range of 10–1200 µg L<sup>−1</sup> and achieving a low detection limit of 3.55 μg L<sup>−1</sup>. Finally, good practicability was verified by application of the method in milk sample analysis.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"213 ","pages":"Article 113650"},"PeriodicalIF":4.9,"publicationDate":"2025-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143844889","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Islam M. Mostafa , Abdallah M. Zeid , Abdelfattah Hassan , Abobakr A. Mohamed
{"title":"Greenness, blueness, and whiteness evaluation of a density functional theory-validated photoinduced electron transfer deactivation protocol for sensitive fluorescence determination of butenafine","authors":"Islam M. Mostafa , Abdallah M. Zeid , Abdelfattah Hassan , Abobakr A. Mohamed","doi":"10.1016/j.microc.2025.113639","DOIUrl":"10.1016/j.microc.2025.113639","url":null,"abstract":"<div><div>In this study, we introduce a photoinduced electron transfer (PET)-off fluorescence enhancement strategy for the sensitive detection of butenafine hydrochloride (BFH), an antifungal agent exhibiting inherently low fluorescence due to PET effects. Protonation of BFH’s tertiary amine moiety effectively suppressed the PET pathway, resulting in a remarkable fluorescence enhancement. Density Functional Theory (DFT) calculations validated this mechanism, revealing distinct shifts in the highest occupied molecular orbital (HOMO) and lowest unoccupied molecular orbital (LUMO) energies between protonated and unprotonated BFH states. The developed method demonstrated exceptional analytical performance, achieving a linear detection range of 15.0–150.0 ng/mL and a detection limit of 2.5 ng/mL. Its practical utility was confirmed through the successful quantification of BFH in a commercial antifungal cream, with recoveries of 98.2–101.8 %. Furthermore, the environmental sustainability, applicability, and practicality of this PET-off approach were rigorously evaluated using the Analytical GREEnness (AGREE) metric, Blue Applicability Grade Index (BAGI) tool, and Red-Green-Blue (RGB) whiteness algorithm. These assessments highlighted its alignment with green analytical chemistry principles while maintaining robust performance for routine pharmaceutical quality control. Compared to previously reported chromatographic and electrochemical methods, the developed spectrofluorimetric method offers a rapid, cost-effective, and highly sensitive alternative for BFH determination. The method eliminates the need for expensive derivatization agents, labor-intensive sample preparation, and sophisticated instrumentation, making it an eco-friendly and sustainable method appropriate for routine pharmaceutical quality control. Moreover, this work not only advances fluorescence-based sensing strategies but also establishes a framework for integrating computational validation and multi-criteria sustainability analysis into analytical method development.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"213 ","pages":"Article 113639"},"PeriodicalIF":4.9,"publicationDate":"2025-04-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143835169","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Doga Ekin Orhan , Ahmet Cetinkaya , Eda Nur Aybi , Mehmet Altay Unal , Hasan Nazir , Sibel Aysil Ozkan , Ilker Ates , Burcu Dogan-Topal
{"title":"Evaluation of the interaction mechanism of dsDNA-propofol binding: Electrochemical, thermodynamic, molecular docking studies and comet assay","authors":"Doga Ekin Orhan , Ahmet Cetinkaya , Eda Nur Aybi , Mehmet Altay Unal , Hasan Nazir , Sibel Aysil Ozkan , Ilker Ates , Burcu Dogan-Topal","doi":"10.1016/j.microc.2025.113647","DOIUrl":"10.1016/j.microc.2025.113647","url":null,"abstract":"<div><div>Propofol, a widely used intravenous hypnotic agent, is favored in medical settings due to its rapid onset and short duration of action. This study systematically assessed the interaction between propofol and DNA using voltammetry, fluorescence spectroscopy, molecular docking, and comet assay analysis. The voltammetric peak responses for dGuo and dAdo on the ct-dsDNA biosensor were detected at 0.96 V and 1.23 V, respectively. 4 × 10<sup>−7</sup> mol L<sup>−1</sup> propofol at 300 s were selected as optimal interaction concentration, which significantly reduced the peak currents of dsDNA signals. In the incubation solution, a significant decrease in the peak currents of both dGuo and dAdo was observed in the 1 × 10<sup>−4</sup> mol/L propofol. To analyze the quenching mechanism, experiments were conducted at various temperatures with Stern-Volmer plots using the fluorescence titration method. The decrease in Ksv values as temperature increases suggests an involvement of static quenching. ΔH° < 0 and ΔS° < 0 indicate the hydrogen bonds and van der Waals interactions; ΔG° < 0 and Kb value of 1.26 × 10<sup>6</sup> L.mol<sup>−1</sup> demonstrate spontaneous interactions between propofol and DNA. Iodide quenching studies revealed that propofol may interact with dsDNA by groove binding. In the comet assay, the highest level of DNA damage was observed at 200 μg/ml propofol concentration. In silico studies, it has been supported that propofol binds to specific minor regions on DNA, forming van der Waals interactions.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"213 ","pages":"Article 113647"},"PeriodicalIF":4.9,"publicationDate":"2025-04-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143844890","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Fu Shu , Zhihui Cheng , Gang Yuan , Yuan Qiu , Qi Sun , Hanping He , Genyan Liu
{"title":"A near-infrared fluorescent probe with a self-immolative linker for rapid detection of beta-galactosidase and specific imaging of ovarian cancer cells","authors":"Fu Shu , Zhihui Cheng , Gang Yuan , Yuan Qiu , Qi Sun , Hanping He , Genyan Liu","doi":"10.1016/j.microc.2025.113640","DOIUrl":"10.1016/j.microc.2025.113640","url":null,"abstract":"<div><div>Beta-galactosidase (β-gal) is a vital biological target which is widely used in the diagnosis of ovarian cancers. To date, only a few near-infrared fluorescent probes were successfully applied to monitor β-gal activity both <em>in vitro</em> and <em>in vivo</em>. However, these β-gal probes have disadvantages as poor water-solubility or slow response rate. To overcome these shortcomings, we constructed a novel near-infrared fluorescent probe (<strong>Cy-βgal</strong>) for β-gal tracing by using self-immolative group connected with fluorophore hemicyanine skeleton (<strong>Cy-OH</strong>) and recognition group (D-galactose). As expected, <strong>Cy-βgal</strong> displayed a fast response rate (8 min) to β-gal in water solution containing only 0.1 % DMSO with a fluorescent turn-on model. In addition, <strong>Cy-βgal</strong> exhibited favorable affinity (<em>K</em><sub>m</sub> = 23.51 μM) to β-gal accompanied with high catalytic efficiency (<em>k</em><sub>cat</sub>/<em>K</em><sub>m</sub> = 2.47 μM<sup>−1</sup> s<sup>−1</sup>). Most importantly, <strong>Cy-βgal</strong> was able to specifically distinguish the ovarian cancer cells from lung cancer cells via the red fluorescence imaging signal of endogenous β-gal in living cells, implying that <strong>Cy-βgal</strong> has the potential for the diagnosis of ovarian cancer. It also confirmed that the self-immolative group-based designing strategy is a practical method for the rational design of other types of β-gal fluorescent probes.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"213 ","pages":"Article 113640"},"PeriodicalIF":4.9,"publicationDate":"2025-04-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143847770","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
G.M. S. Souza , R. Debastiani , P. Chytry , M. Knebel , R. Thomaz , L. Amaral , J. F. Dias
{"title":"A simple protocol for the characterization of fraudulent erectile dysfunction medicines using ion beam analytical techniques","authors":"G.M. S. Souza , R. Debastiani , P. Chytry , M. Knebel , R. Thomaz , L. Amaral , J. F. Dias","doi":"10.1016/j.microc.2025.113602","DOIUrl":"10.1016/j.microc.2025.113602","url":null,"abstract":"<div><div>In this work we developed a simple and fast protocol based solely on ion beam analytical techniques for the analysis of erectile dysfunction medicines containing sildenafil and vardenafil as active ingredients. To that end, RBS (Rutherford Backscattering Spectrometry), PIXE (Particle-Induced X-ray Emission) and MeV-SIMS (Secondary Ion Mass Spectrometry) were employed in the analysis of sildenafil citrate (Viagra®), vardenafil hydrochloride (Levitra®) and tadalafil (Cialis®) among other medications. The RBS and PIXE techniques provide information on the concentrations of major and trace elements present in the tablets respectively, while the MeV-SIMS technique was used for the determination of the molecular profile of the samples. The protocol is based on the detection of sulfur present in the tablets through the PIXE technique, while its validation relies on the detection of the active ingredients with the MeV-SIMS technique.</div><div>The results confirm that the protocol is quite suitable for the discrimination of different sildenafil- and vardenafil-based medicines. On the other hand, this protocol cannot be used for the study of tadalafil-based medicines since no detectable element by PIXE is present in its active ingredient.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"213 ","pages":"Article 113602"},"PeriodicalIF":4.9,"publicationDate":"2025-04-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143844807","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}