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Electroactive Fe-MOFs as an internal reference for ratiometric electrochemical sensing of 17β-estradiol with reinforcement of graphene nanosheets
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-04-15 DOI: 10.1016/j.microc.2025.113650
Chen Yang , Zhe Zhuang , Xiyu Zhang , Ziyi Ren , Danling Sun , Ping Wu , Jinzhou Liu , Wei Wu , Xuerong Chen
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−1 and achieving a low detection limit of 3.55 μg L−1. Finally, good practicability was verified by application of the method in milk sample analysis.
比率策略对于提高电化学传感器的重现性和可靠性非常有效。本文采用了一种新型内参探针,即铁基 MOFs(MIL-101),由于其具有明显的铁氧化行为,无需使用广泛使用的固定电活性小分子升汞,即可提供参比信号。此外,通过引入石墨烯纳米片(GS),得到的 MIL-101/GS 复合材料在电化学活性表面、电子转移动力学和吸附性能方面都有显著增强。与单个成分相比,由于 MIL-101 和 GS 的共同作用,复合材料对铁和 17β- 雌二醇(E2)的氧化信号都有明显改善。在双信号输出模型的基础上,一种灵敏可靠的 E2 比率电化学传感器被轻松构建出来,其线性范围宽至 10-1200 µg L-1,检测限低至 3.55 μg L-1。最后,该方法在牛奶样品分析中的应用验证了其良好的实用性。
{"title":"Electroactive Fe-MOFs as an internal reference for ratiometric electrochemical sensing of 17β-estradiol with reinforcement of graphene nanosheets","authors":"Chen Yang ,&nbsp;Zhe Zhuang ,&nbsp;Xiyu Zhang ,&nbsp;Ziyi Ren ,&nbsp;Danling Sun ,&nbsp;Ping Wu ,&nbsp;Jinzhou Liu ,&nbsp;Wei Wu ,&nbsp;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}
引用次数: 0
Aldehydes determination in edible oil samples employing 1-Naphthalenyl hydrazine as derivatizing agent followed by HPLC-FLD
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-04-15 DOI: 10.1016/j.microc.2025.113658
Jorge Lopez-Tellez , Israel S. Ibarra , Eva M. Santos , Alicia C. Mondragon-Portocarrero , Jose A. Rodriguez
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−1. 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.
食品中醛类的形成是加工或降解步骤的结果。这些化合物会导致口感、风味、气味、颜色、质地和外观变差,营养价值也会受到影响,而且可能对健康产生不良影响。在这种情况下,对它们进行分析对质量控制至关重要。因此,本研究提出了一种以 1-萘肼为衍生剂的荧光衍生方法,用于测定戊醛、己醛、庚醛、辛醛、壬醛和癸醛,然后进行 HPLC-FLD,检测限在 4.0-6.2 µg L-1 之间。通过全因子和箱-贝肯实验设计对衍生化过程进行了优化,随后进行了验证,并将其应用于食用油样品中醛的测定。所提出的衍生化方法高效、精确(以相对标准偏差表示为 10%)、准确(92.57-109.68%)。与现有的使用 2,4-二硝基苯肼、二(吡咯-2-基)甲酮或其他衍生化合物的方法相比,所提出的衍生方法是一种有竞争力的替代方法。此外,荧光法的检测限与质谱法色谱系统的检测限相当。该方法可用于定量检测长链醛的总含量,在食品质量控制方面具有良好的前景,因此可用于多种醛类和复杂样品。
{"title":"Aldehydes determination in edible oil samples employing 1-Naphthalenyl hydrazine as derivatizing agent followed by HPLC-FLD","authors":"Jorge Lopez-Tellez ,&nbsp;Israel S. Ibarra ,&nbsp;Eva M. Santos ,&nbsp;Alicia C. Mondragon-Portocarrero ,&nbsp;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 &lt;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}
引用次数: 0
Greenness, blueness, and whiteness evaluation of a density functional theory-validated photoinduced electron transfer deactivation protocol for sensitive fluorescence determination of butenafine
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-04-14 DOI: 10.1016/j.microc.2025.113639
Islam M. Mostafa , Abdallah M. Zeid , Abdelfattah Hassan , Abobakr A. Mohamed
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.
{"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 ,&nbsp;Abdallah M. Zeid ,&nbsp;Abdelfattah Hassan ,&nbsp;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}
引用次数: 0
Evaluation of the interaction mechanism of dsDNA-propofol binding: Electrochemical, thermodynamic, molecular docking studies and comet assay
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-04-14 DOI: 10.1016/j.microc.2025.113647
Doga Ekin Orhan , Ahmet Cetinkaya , Eda Nur Aybi , Mehmet Altay Unal , Hasan Nazir , Sibel Aysil Ozkan , Ilker Ates , Burcu Dogan-Topal
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 × 10−7 mol L−1 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 × 10−4 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 × 106 L.mol−1 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.
丙泊酚是一种广泛使用的静脉催眠药,因其起效快、作用时间短而在医疗领域备受青睐。本研究采用伏安法、荧光光谱法、分子对接法和彗星试验分析法系统地评估了丙泊酚与 DNA 之间的相互作用。dGuo 和 dAdo 在 ct-dsDNA 生物传感器上的伏安峰响应分别为 0.96 V 和 1.23 V。选择 4 × 10-7 mol L-1 丙泊酚在 300 秒内作为最佳相互作用浓度,可显著降低 dsDNA 信号的峰值电流。在孵育液中,观察到 1 × 10-4 mol/L 异丙酚可显著降低 dGuo 和 dAdo 的峰值电流。为了分析淬灭机制,在不同温度下使用荧光滴定法绘制了 Stern-Volmer 图。Ksv 值随着温度的升高而降低,这表明其中有静态淬火的参与。ΔH° < 0 和 ΔS° < 0 表示氢键和范德华相互作用;ΔG° < 0 和 Kb 值 1.26 × 106 L.mol-1 表明异丙酚和 DNA 之间存在自发相互作用。碘化物淬灭研究表明,异丙酚可能通过沟结合与 dsDNA 发生相互作用。在彗星试验中,浓度为 200 μg/ml 的异丙酚对 DNA 的损伤程度最高。硅学研究证实,异丙酚与 DNA 上的特定次要区域结合,形成范德华相互作用。
{"title":"Evaluation of the interaction mechanism of dsDNA-propofol binding: Electrochemical, thermodynamic, molecular docking studies and comet assay","authors":"Doga Ekin Orhan ,&nbsp;Ahmet Cetinkaya ,&nbsp;Eda Nur Aybi ,&nbsp;Mehmet Altay Unal ,&nbsp;Hasan Nazir ,&nbsp;Sibel Aysil Ozkan ,&nbsp;Ilker Ates ,&nbsp;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° &lt; 0 and ΔS° &lt; 0 indicate the hydrogen bonds and van der Waals interactions; ΔG° &lt; 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}
引用次数: 0
A near-infrared fluorescent probe with a self-immolative linker for rapid detection of beta-galactosidase and specific imaging of ovarian cancer cells
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-04-14 DOI: 10.1016/j.microc.2025.113640
Fu Shu , Zhihui Cheng , Gang Yuan , Yuan Qiu , Qi Sun , Hanping He , Genyan Liu
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 in vitro and in vivo. 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 (Cy-βgal) for β-gal tracing by using self-immolative group connected with fluorophore hemicyanine skeleton (Cy-OH) and recognition group (D-galactose). As expected, Cy-βgal 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, Cy-βgal exhibited favorable affinity (Km = 23.51 μM) to β-gal accompanied with high catalytic efficiency (kcat/Km = 2.47 μM−1 s−1). Most importantly, Cy-βgal 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 Cy-βgal 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.
{"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 ,&nbsp;Zhihui Cheng ,&nbsp;Gang Yuan ,&nbsp;Yuan Qiu ,&nbsp;Qi Sun ,&nbsp;Hanping He ,&nbsp;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}
引用次数: 0
A simple protocol for the characterization of fraudulent erectile dysfunction medicines using ion beam analytical techniques 利用离子束分析技术表征勃起功能障碍假药的简单方案
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-04-14 DOI: 10.1016/j.microc.2025.113602
G.M. S. Souza , R. Debastiani , P. Chytry , M. Knebel , R. Thomaz , L. Amaral , J. F. Dias
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.
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.
{"title":"A simple protocol for the characterization of fraudulent erectile dysfunction medicines using ion beam analytical techniques","authors":"G.M. S. Souza ,&nbsp;R. Debastiani ,&nbsp;P. Chytry ,&nbsp;M. Knebel ,&nbsp;R. Thomaz ,&nbsp;L. Amaral ,&nbsp;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}
引用次数: 0
Machine learning-integrated biomimetic electronic noses: Future perspectives 机器学习集成生物仿真电子鼻:未来展望
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-04-14 DOI: 10.1016/j.microc.2025.113638
Taeha Lee , Jun Yu , Sang Won Lee , Seung Hyeon Oh , Dain Kang , Hyunmok Son , Han-Jeong Hwang , Jae Hyun You , Gyudo Lee
The electronic nose (E-nose) is an innovative device that mimics the human sense of smell. E-noses are used for effective detection and discrimination between complex odors. Compared to traditional odor detection methods, E-nose technology employs a sensor array that differentiates and measures airborne smells through a combination of electrical signals generated by the sensor array when detecting odors. In addition, the incorporation of machine learning for data processing has enhanced the sensitivity and selectivity of odor molecular detection. However, certain limitations exist, such as a limited range of detectable odor molecules and low analytical accuracy for similar compounds, which challenge the claim that E-noses can fully mimic human olfaction. In this paper, we provides a general overview of the E-nose structure and its operating principles, as well as a summary of recent research and practical constraints in detecting volatile organic compounds. Moreover, this review paper discusses the future development of biomimetic E-noses in conjunction with other technologies and describes their potential commercial applications, including through E-commerce platforms. The critical review contributes to the E-nose literature by offering insights into how the E-nose device can solve real-world problems and by proposing directions for future advancement.
{"title":"Machine learning-integrated biomimetic electronic noses: Future perspectives","authors":"Taeha Lee ,&nbsp;Jun Yu ,&nbsp;Sang Won Lee ,&nbsp;Seung Hyeon Oh ,&nbsp;Dain Kang ,&nbsp;Hyunmok Son ,&nbsp;Han-Jeong Hwang ,&nbsp;Jae Hyun You ,&nbsp;Gyudo Lee","doi":"10.1016/j.microc.2025.113638","DOIUrl":"10.1016/j.microc.2025.113638","url":null,"abstract":"<div><div>The electronic nose (E-nose) is an innovative device that mimics the human sense of smell. E-noses are used for effective detection and discrimination between complex odors. Compared to traditional odor detection methods, E-nose technology employs a sensor array that differentiates and measures airborne smells through a combination of electrical signals generated by the sensor array when detecting odors. In addition, the incorporation of machine learning for data processing has enhanced the sensitivity and selectivity of odor molecular detection. However, certain limitations exist, such as a limited range of detectable odor molecules and low analytical accuracy for similar compounds, which challenge the claim that E-noses can fully mimic human olfaction. In this paper, we provides a general overview of the E-nose structure and its operating principles, as well as a summary of recent research and practical constraints in detecting volatile organic compounds. Moreover, this review paper discusses the future development of biomimetic E-noses in conjunction with other technologies and describes their potential commercial applications, including through E-commerce platforms. The critical review contributes to the E-nose literature by offering insights into how the E-nose device can solve real-world problems and by proposing directions for future advancement.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"213 ","pages":"Article 113638"},"PeriodicalIF":4.9,"publicationDate":"2025-04-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143844809","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}
引用次数: 0
Self-powered photoelectrochemical sensor based on porous carbon nitride by a simple precursor pretreatment strategy as photoanode for Pb2+ detection
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-04-13 DOI: 10.1016/j.microc.2025.113648
Chunhui Zhao, Rui Wang, Han Yin, Bao Chang, Xiuli Dong, Shiyu Wang, Meiyu Yang, Jiali Yang, Yang Zhao, Huan Wang
Ensuring food safety and environmental protection requires the rapid detection of lead ion (Pb2+), an additive frequently utilised in industrial and domestic applications. Herein, a self-powered photoelectrochemical sensor (SPES) was constructed by integrating a photocatalytic hydrogen peroxide fuel cell (PFC) with an electrochemical sensor. Unlike traditional electrochemical sensor, this SPES relies not only on the band gap of the photoanode but also on the efficient separation and transportation of the photogenerated carriers. The porous carbon nitride (HE-CN) was prepared using a simple precursor pretreatment strategy, which provides more reactive sites and achieves more efficient separation and transport of photogenerated carriers than bulk carbon nitride (CN) produced by conventional method. Using the mechanism of photoanode adsorption of Pb2+, HE-CN was designed as the photoanode material,which greatly enhances the output energy of the SPES. Under ideal test conditions, the SPES demonstrated a low detection limit of 0.42 nM (Signal-to-noise ratio (S/N) = 3) for Pb2+ and a linear response concentration range from 0.01 to 1.5 μM, with a correlation coefficient of 0.9918, and the spiked recovery rate is between 96.2 % and 106.8 %. Therefore, the SPES platform exhibits excellent stability, good reproducibility,as well as a high sensitivity in detecting Pb2+.
{"title":"Self-powered photoelectrochemical sensor based on porous carbon nitride by a simple precursor pretreatment strategy as photoanode for Pb2+ detection","authors":"Chunhui Zhao,&nbsp;Rui Wang,&nbsp;Han Yin,&nbsp;Bao Chang,&nbsp;Xiuli Dong,&nbsp;Shiyu Wang,&nbsp;Meiyu Yang,&nbsp;Jiali Yang,&nbsp;Yang Zhao,&nbsp;Huan Wang","doi":"10.1016/j.microc.2025.113648","DOIUrl":"10.1016/j.microc.2025.113648","url":null,"abstract":"<div><div>Ensuring food safety and environmental protection requires the rapid detection of lead ion (Pb<sup>2+</sup>), an additive frequently utilised in industrial and domestic applications. Herein, a self-powered photoelectrochemical sensor (SPES) was constructed by integrating a photocatalytic hydrogen peroxide fuel cell (PFC) with an electrochemical sensor. Unlike traditional electrochemical sensor, this SPES relies not only on the band gap of the photoanode but also on the efficient separation and transportation of the photogenerated carriers. The porous carbon nitride (HE-CN) was prepared using a simple precursor pretreatment strategy, which provides more reactive sites and achieves more efficient separation and transport of photogenerated carriers than bulk carbon nitride (CN) produced by conventional method. Using the mechanism of photoanode adsorption of Pb<sup>2+</sup>, HE-CN was designed as the photoanode material,which greatly enhances the output energy of the SPES. Under ideal test conditions, the SPES demonstrated a low detection limit of 0.42 nM (Signal-to-noise ratio (S/N) = 3) for Pb<sup>2+</sup> and a linear response concentration range from 0.01 to 1.5 μM, with a correlation coefficient of 0.9918, and the spiked recovery rate is between 96.2 % and 106.8 %. Therefore, the SPES platform exhibits excellent stability, good reproducibility,as well as a high sensitivity in detecting Pb<sup>2+</sup>.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"213 ","pages":"Article 113648"},"PeriodicalIF":4.9,"publicationDate":"2025-04-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143839543","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}
引用次数: 0
Polybrominated diphenyl ethers in household dust of breastfeeding mothers: Exposure levels and risk assessment
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-04-12 DOI: 10.1016/j.microc.2025.113635
Esther Fuentes-Ferragud , Pablo Miralles , Antonio López , María Ibáñez , Clara Coscollà
In the present study, 55 household dust samples were collected from the homes of breastfeeding mothers from the Valencian Region (Spain) to analyze the presence of 25 polybrominated diphenyl ethers (PBDEs). The extraction method was based on microwave-assisted extraction (MAE) followed by acid digestion and solid phase extraction clean-up steps. The overall analytical method, using gas chromatography coupled to high resolution mass spectrometry (GC-HRMS), was optimized and validated through, both, in-house validation and the use of a certified reference material (CRM). Limits of quantification (LOQ) ranged from 0.38 to 2 µg kg−1. PBDEs levels were determined in household dust, with concentrations ranging from 0.40 to 302.7 µg kg−1 for mono-, di-, tri-, tetra-, penta-, hexa-, hepta- and octa-BDEs, and from 2.18 to 60664 µg kg−1 for nona- and deca-BDEs, with BDE-209 being the most abundant and frequently detected congener. A risk assessment was conducted based on dust ingestion for mothers, toddlers and children. No potential health risk was identified, except for BDE-206 and BDE-207, which posed a concern for toddlers and infants. Finally, associations between PBDEs levels and various factors, such as ventilation, furniture, type of flooring, geographical location and the number of electronic devices, were found to influence PBDEs levels in household dust.
{"title":"Polybrominated diphenyl ethers in household dust of breastfeeding mothers: Exposure levels and risk assessment","authors":"Esther Fuentes-Ferragud ,&nbsp;Pablo Miralles ,&nbsp;Antonio López ,&nbsp;María Ibáñez ,&nbsp;Clara Coscollà","doi":"10.1016/j.microc.2025.113635","DOIUrl":"10.1016/j.microc.2025.113635","url":null,"abstract":"<div><div>In the present study, 55 household dust samples were collected from the homes of breastfeeding mothers from the Valencian Region (Spain) to analyze the presence of 25 polybrominated diphenyl ethers (PBDEs). The extraction method was based on microwave-assisted extraction (MAE) followed by acid digestion and solid phase extraction clean-up steps. The overall analytical method, using gas chromatography coupled to high resolution mass spectrometry (GC-HRMS), was optimized and validated through, both, in-house validation and the use of a certified reference material (CRM). Limits of quantification (LOQ) ranged from 0.38 to 2 µg kg<sup>−1</sup>. PBDEs levels were determined in household dust, with concentrations ranging from 0.40 to 302.7 µg kg<sup>−1</sup> for mono-, di-, tri-, tetra-, penta-, hexa-, hepta- and octa-BDEs, and from 2.18 to 60664 µg kg<sup>−1</sup> for nona- and deca-BDEs, with BDE-209 being the most abundant and frequently detected congener. A risk assessment was conducted based on dust ingestion for mothers, toddlers and children. No potential health risk was identified, except for BDE-206 and BDE-207, which posed a concern for toddlers and infants. Finally, associations between PBDEs levels and various factors, such as ventilation, furniture, type of flooring, geographical location and the number of electronic devices, were found to influence PBDEs levels in household dust.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"213 ","pages":"Article 113635"},"PeriodicalIF":4.9,"publicationDate":"2025-04-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143844802","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}
引用次数: 0
Afterglow time-resolved lateral flow immunoassay platform with a low-cost handheld reader for on-site detection of methamphetamine 带有低成本手持读取器的余辉时间分辨横向流动免疫分析平台,用于现场检测甲基苯丙胺
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2025-04-12 DOI: 10.1016/j.microc.2025.113615
Haolan Yuan , Jie Cheng , Jiuchuan Guo , Diangeng Li , Jinhong Guo
Methylamphetamine (methamphetamine, MET) is a highly addictive drug worldwide. In drug abuse screening, point-of-care detection is crucial for addiction treatment and rehabilitation centers, as well as law enforcement agencies. Among various point-of-care detection methods, lateral flow immunoassay (LFIA) has garnered widespread attention due to its unique advantages of ease of use and speed. However, conventional colloidal gold-based LFIA can only perform qualitative or semi-quantitative detection, while most quantitative LFIAs based on optical nanoprobes require expensive equipment to read signals, limiting broader adoption. In this study, we developed a novel afterglow time-resolved fluorescence LFIA (AG-LFIA) technology that enables on-site quantitative detection of MET in urine through a custom-developed miniature sensing device. Considering product development and commercialization, a one-step coprecipitation method and an in-situ self-assembly method were established to prepare afterglow probes in large quantities for scalable production. The proposed AG-LFIA sensing strategy effectively eliminates interference from endogenous biological signals and excitation light. Furthermore, leveraging the afterglow properties, an integrated fluorescence signal amplification and collection strategy was introduced, which improves the signal-to-noise ratio and obviates the requirement for intricate optical configurations and filters in traditional optical readers. As a result, the AG-LFIA achieved an MET detection range of 4–10000 ng/mL, with a limit of quantification (LoQ) of 4 ng/mL and a detection time of 10 min. The AG-LFIA is user-friendly, highly sensitive, and accurate, making it an effective candidate for real-time drug abuse screening.
{"title":"Afterglow time-resolved lateral flow immunoassay platform with a low-cost handheld reader for on-site detection of methamphetamine","authors":"Haolan Yuan ,&nbsp;Jie Cheng ,&nbsp;Jiuchuan Guo ,&nbsp;Diangeng Li ,&nbsp;Jinhong Guo","doi":"10.1016/j.microc.2025.113615","DOIUrl":"10.1016/j.microc.2025.113615","url":null,"abstract":"<div><div>Methylamphetamine (methamphetamine, MET) is a highly addictive drug worldwide. In drug abuse screening, point-of-care detection is crucial for addiction treatment and rehabilitation centers, as well as law enforcement agencies. Among various point-of-care detection methods, lateral flow immunoassay (LFIA) has garnered widespread attention due to its unique advantages of ease of use and speed. However, conventional colloidal gold-based LFIA can only perform qualitative or semi-quantitative detection, while most quantitative LFIAs based on optical nanoprobes require expensive equipment to read signals, limiting broader adoption. In this study, we developed a novel afterglow time-resolved fluorescence LFIA (AG-LFIA) technology that enables on-site quantitative detection of MET in urine through a custom-developed miniature sensing device. Considering product development and commercialization, a one-step coprecipitation method and an in-situ self-assembly method were established to prepare afterglow probes in large quantities for scalable production. The proposed AG-LFIA sensing strategy effectively eliminates interference from endogenous biological signals and excitation light. Furthermore, leveraging the afterglow properties, an integrated fluorescence signal amplification and collection strategy was introduced, which improves the signal-to-noise ratio and obviates the requirement for intricate optical configurations and filters in traditional optical readers. As a result, the AG-LFIA achieved an MET detection range of 4–10000 ng/mL, with a limit of quantification (LoQ) of 4 ng/mL and a detection time of 10 min. The AG-LFIA is user-friendly, highly sensitive, and accurate, making it an effective candidate for real-time drug abuse screening.</div></div>","PeriodicalId":391,"journal":{"name":"Microchemical Journal","volume":"213 ","pages":"Article 113615"},"PeriodicalIF":4.9,"publicationDate":"2025-04-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143835167","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}
引用次数: 0
期刊
Microchemical Journal
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