Pub Date : 2025-01-17DOI: 10.1016/j.talo.2025.100410
Bartosz Marciniak , Paweł Georgiev , Dagmara Kroll , Szymon Ulenberg , Tomasz Bączek , Mariusz Belka
Our study investigated the impact of 3D-printed sorbent device geometry on extraction of benzodiazepines (BZD). Utilizing additive manufacturing (AM), we created devices with varying shapes and sizes, including cylinders and volumetric lattices. The sorbent material was a suspension of C18-coated silica gel in a photocurable resin. Our findings revealed that device geometry significantly influenced extraction efficiency. Area, internal shape, and size all impacted BZD recovery. Volumetric lattices, particularly gyroid and x-cell shapes, outperformed cylinders. Larger devices generally led to higher absolute recovery, but standardization per unit area showed smaller devices to be more efficient. These results provide valuable insights for designing optimized sorbent devices, contributing to advancements in solid-phase extraction.
{"title":"Comprehensive experimental study on the impact of size and geometry of 3D-printed devices on solid-phase extraction efficiency and reproducibility","authors":"Bartosz Marciniak , Paweł Georgiev , Dagmara Kroll , Szymon Ulenberg , Tomasz Bączek , Mariusz Belka","doi":"10.1016/j.talo.2025.100410","DOIUrl":"10.1016/j.talo.2025.100410","url":null,"abstract":"<div><div>Our study investigated the impact of 3D-printed sorbent device geometry on extraction of benzodiazepines (BZD). Utilizing additive manufacturing (AM), we created devices with varying shapes and sizes, including cylinders and volumetric lattices. The sorbent material was a suspension of C18-coated silica gel in a photocurable resin. Our findings revealed that device geometry significantly influenced extraction efficiency. Area, internal shape, and size all impacted BZD recovery. Volumetric lattices, particularly gyroid and x-cell shapes, outperformed cylinders. Larger devices generally led to higher absolute recovery, but standardization per unit area showed smaller devices to be more efficient. These results provide valuable insights for designing optimized sorbent devices, contributing to advancements in solid-phase extraction.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"11 ","pages":"Article 100410"},"PeriodicalIF":4.1,"publicationDate":"2025-01-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143159209","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-01-16DOI: 10.1016/j.talo.2025.100409
Tsutomu Miura
Instrumental neutron activation analysis (INAA) is a valuable technique for quantifying F; however, it is associated with significant measurement uncertainty, which can be reduced by combining INAA with the internal standard method. In this study, known amounts of Sc were added to both samples and calibration standards to compensate for variations in the fluence rates of the irradiated neutrons and measurements of the γ-rays. The 46mSc produced during neutron irradiation was used as the internal standard. Data were collected using two approaches: a single irradiation for 5 s followed by a 10 s γ-ray measurement, and a cyclic method involving five repetitions of the single irradiation and γ-ray measurements. Normalization of the counting rate using the internal standard effectively eliminated day-to-day variations, and a reliable relationship was established between the normalized signal and the amount of F. The proposed method produced a robust and highly linear calibration plot, enabling the accurate quantification of the mass fraction of F. The analytical performance of the proposed method was validated using certified reference materials before using it to quantify the mass fraction of F in commercially available synthetic polymer resins. The cyclic irradiation method, which required approximately 30 min for measurement, yielded a lower expanded uncertainty in the mass fraction of F compared with the single irradiation method, in which measurements were completed within 30 s. Consequently, the single irradiation method was more suitable for screening, whereas the cyclic irradiation method was more suitable for the precise quantification of F.
{"title":"Total fluorine analysis in solid samples by instrumental neutron activation analysis coupled with the internal standard method","authors":"Tsutomu Miura","doi":"10.1016/j.talo.2025.100409","DOIUrl":"10.1016/j.talo.2025.100409","url":null,"abstract":"<div><div>Instrumental neutron activation analysis (INAA) is a valuable technique for quantifying F; however, it is associated with significant measurement uncertainty, which can be reduced by combining INAA with the internal standard method. In this study, known amounts of Sc were added to both samples and calibration standards to compensate for variations in the fluence rates of the irradiated neutrons and measurements of the γ-rays. The <sup>46m</sup>Sc produced during neutron irradiation was used as the internal standard. Data were collected using two approaches: a single irradiation for 5 s followed by a 10 s γ-ray measurement, and a cyclic method involving five repetitions of the single irradiation and γ-ray measurements. Normalization of the counting rate using the internal standard effectively eliminated day-to-day variations, and a reliable relationship was established between the normalized signal and the amount of F. The proposed method produced a robust and highly linear calibration plot, enabling the accurate quantification of the mass fraction of F. The analytical performance of the proposed method was validated using certified reference materials before using it to quantify the mass fraction of F in commercially available synthetic polymer resins. The cyclic irradiation method, which required approximately 30 min for measurement, yielded a lower expanded uncertainty in the mass fraction of F compared with the single irradiation method, in which measurements were completed within 30 s. Consequently, the single irradiation method was more suitable for screening, whereas the cyclic irradiation method was more suitable for the precise quantification of F.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"11 ","pages":"Article 100409"},"PeriodicalIF":4.1,"publicationDate":"2025-01-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143159207","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
We studied the gas-sensing properties of Li-decorated C20 nanocage and its derivatives, presenting these materials as novel candidates for sensing applications. The derivatives of C20 considered are either B-substituted, N-substituted or B and N co-substituted C20 Nanocages. Toxic gases H2S and NH3, were selected for evaluation. Out of 15 derivatives analysed, 10 were confirmed to be stable for Li-doping and gas sensing application. The C12N8 nanocage demonstrating the strongest Li-anchoring, characterized by a high Li-binding energy of 3.81 eV. The Li-decoration introduced spin polarization near the Fermi level, reflected in asymmetric spin-up and spin-down states, which indicated the magnetic nature of the resulting complexes. Substantial changes in the electronic structure of the nanocages upon interaction with H2S and NH3 molecules are observed, both of which were found to adsorb favourably over a broad temperature and pressure range. H2S molecule was observed to undergo physisorption, while NH3 exhibited strong chemisorption across all the nanocages. Recovery time analysis highlighted that all nanocages displayed practical recovery times for H2S, with the C10B10 nanocage showing the shortest recovery time, emphasizing its potential as a highly efficient sensor for H2S detection. The designed nanocages show better gas sensing performance for H2S gas molecule than NH3.
{"title":"Li-doped C20 nanocage and its derivatives for gas sensing application: A density functional theory study","authors":"Poonam Parkar , Mohsen Doust Mohammadi , Ajay Chaudhari","doi":"10.1016/j.talo.2025.100408","DOIUrl":"10.1016/j.talo.2025.100408","url":null,"abstract":"<div><div>We studied the gas-sensing properties of Li-decorated C<sub>20</sub> nanocage and its derivatives, presenting these materials as novel candidates for sensing applications. The derivatives of C<sub>20</sub> considered are either B-substituted, N-substituted or B and N co-substituted C<sub>20</sub> Nanocages. Toxic gases H<sub>2</sub>S and NH<sub>3</sub>, were selected for evaluation. Out of 15 derivatives analysed, 10 were confirmed to be stable for Li-doping and gas sensing application. The C<sub>12</sub>N<sub>8</sub> nanocage demonstrating the strongest Li-anchoring, characterized by a high Li-binding energy of 3.81 eV. The Li-decoration introduced spin polarization near the Fermi level, reflected in asymmetric spin-up and spin-down states, which indicated the magnetic nature of the resulting complexes. Substantial changes in the electronic structure of the nanocages upon interaction with H<sub>2</sub>S and NH<sub>3</sub> molecules are observed, both of which were found to adsorb favourably over a broad temperature and pressure range. H<sub>2</sub>S molecule was observed to undergo physisorption, while NH<sub>3</sub> exhibited strong chemisorption across all the nanocages. Recovery time analysis highlighted that all nanocages displayed practical recovery times for H<sub>2</sub>S, with the C<sub>10</sub>B<sub>10</sub> nanocage showing the shortest recovery time, emphasizing its potential as a highly efficient sensor for H<sub>2</sub>S detection. The designed nanocages show better gas sensing performance for H<sub>2</sub>S gas molecule than NH<sub>3</sub>.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"11 ","pages":"Article 100408"},"PeriodicalIF":4.1,"publicationDate":"2025-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143159204","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The rhizome of Zingiber ottensii Valeton (ZOT), commonly known as Phlai Dum, has been long used in Thai traditional medicine for treatment of wounds, flatulence, peptic ulcers and muscle pain. Moreover, this plant, known to contain zerumbone as a major bioactive component, has recently gained considerable attention due to its diverse pharmacological properties, such as anti-inflammatory, anticancer, antimicrobial, and antioxidant activities. Thus, accurate and reliable zerumbone quantification is crucial for ensuring the quality, consistency, and efficacy of the plant materials and preparations. To our knowledge, a specific method for routine analysis of zerumbone in the ZOT rhizomes and extracts is not yet well-established. In addition, despite exiting methods (e.g. HPLC and UHPLC) for the quantification of zerumbone in various plant and product, the application of these methods may not be suitable for quantifying the content of zerumbone in the ZOT rhizomes and extracts due to the difference in phytochemical constituents and complexity of samples. Therefore, in this study, we aimed to develop and validate an HPLC analytical method that could accurately determine zerumbone content in the ethanolic extract of ZOT rhizome. The results indicated that the developed HPLC method complied with the ICH acceptance criteria. The method expressed a specificity to zerumbone with a high linearity in the range of 10 to 1000 µg/mL (R2 > 0.999). The LOD and LOQ values were 2.89 and 8.75 µg/mL, respectively. The method demonstrated excellent precision, with a relative standard deviation (%RSD) lower than 2, as well as exhibited a high degree of accuracy within an acceptable recovery range of 95–105 %. Additionally, the HPLC method can also be applied to analyze a variation of zerumbone in ZOT raw materials obtained from six different locations in Thailand, which was found to be within the range of 4.30 to 10.46 mg/g of crude powder. This method, therefore, will be very useful for selecting good raw materials of ZOT and standardizing its extracts for future applications.
{"title":"Validation of HPLC method for quantitative determination of zerumbone in the rhizome of Zingiber ottensii Valeton","authors":"Patcharaporn Muanrit , Saovapak Poomirat , Intouch Sakpakdeejaroen","doi":"10.1016/j.talo.2025.100405","DOIUrl":"10.1016/j.talo.2025.100405","url":null,"abstract":"<div><div>The rhizome of <em>Zingiber ottensii</em> Valeton (ZOT), commonly known as Phlai Dum, has been long used in Thai traditional medicine for treatment of wounds, flatulence, peptic ulcers and muscle pain. Moreover, this plant, known to contain zerumbone as a major bioactive component, has recently gained considerable attention due to its diverse pharmacological properties, such as anti-inflammatory, anticancer, antimicrobial, and antioxidant activities. Thus, accurate and reliable zerumbone quantification is crucial for ensuring the quality, consistency, and efficacy of the plant materials and preparations. To our knowledge, a specific method for routine analysis of zerumbone in the ZOT rhizomes and extracts is not yet well-established. In addition, despite exiting methods (e.g. HPLC and UHPLC) for the quantification of zerumbone in various plant and product, the application of these methods may not be suitable for quantifying the content of zerumbone in the ZOT rhizomes and extracts due to the difference in phytochemical constituents and complexity of samples. Therefore, in this study, we aimed to develop and validate an HPLC analytical method that could accurately determine zerumbone content in the ethanolic extract of ZOT rhizome. The results indicated that the developed HPLC method complied with the ICH acceptance criteria. The method expressed a specificity to zerumbone with a high linearity in the range of 10 to 1000 µg/mL (R<sup>2</sup> > 0.999). The LOD and LOQ values were 2.89 and 8.75 µg/mL, respectively. The method demonstrated excellent precision, with a relative standard deviation (%RSD) lower than 2, as well as exhibited a high degree of accuracy within an acceptable recovery range of 95–105 %. Additionally, the HPLC method can also be applied to analyze a variation of zerumbone in ZOT raw materials obtained from six different locations in Thailand, which was found to be within the range of 4.30 to 10.46 mg/g of crude powder. This method, therefore, will be very useful for selecting good raw materials of ZOT and standardizing its extracts for future applications.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"11 ","pages":"Article 100405"},"PeriodicalIF":4.1,"publicationDate":"2025-01-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143159138","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-01-13DOI: 10.1016/j.talo.2025.100406
Amr M. Mahmoud , Nariman A. El-Ragehy , Maha A. Hegazy , Samia A. Tawfik , Ghada A. Sedik
Currently, the global push for eco-friendly analytical techniques has altered the priorities of analytical methodologies in accordance with their level of adherence to the principles of green analytical chemistry. Herein, sustainable, sensitive, accurate and cost-effective core-shell molecularly imprinted polymer (MIP) has been developed for the determination of trazodone hydrochloride. It is a widely prescribed medication primarily used to treat depression, anxiety and insomnia. Its detection is significant for ensuring effective therapeutic drug monitoring as it has a narrow therapeutic window in addition to optimize dosages, prevent toxicity, and enhance treatment outcomes. MIP with a uniform core shell structure was prepared where the shell was combined onto the surface of silica nanoparticles by copolymerizing ethylene glycol dimethacrylate together with methacrylic acid in the presence of trazodone hydrochloride. The core consists of silica nanoparticles developed by Stöber method. The core-shell MIP was then embedded as ionophore into the polyvinyl chloride liquid membrane. A linear relationship was found over a dynamic range of 1.0 × 10 –6 -1.0 × 10 – 2 M with LOD of 6.0 × 10–7 M and Nernstian slope of 56.70 mV/decade. The developed method was successfully applied for determination of trazodone hydrochloride in its tablet dosage form with mean percentage recovery of 103.08%. Moreover, the suggested sensor has a significant potential to monitor patients’ plasma level to guarantee drug safety and effectiveness. Additionally, three different approaches namely; Analytical EcoScale, Analytical GREEnness metric approach and finally, the most recent one; Red-Green-Blue model were applied to evaluate the greenness and whiteness profile of the developed method.
{"title":"Electrochemical sensor doped with core-shell structured molecularly imprinted polymer proposed for therapeutic drug monitoring of trazodone hydrochloride","authors":"Amr M. Mahmoud , Nariman A. El-Ragehy , Maha A. Hegazy , Samia A. Tawfik , Ghada A. Sedik","doi":"10.1016/j.talo.2025.100406","DOIUrl":"10.1016/j.talo.2025.100406","url":null,"abstract":"<div><div>Currently, the global push for eco-friendly analytical techniques has altered the priorities of analytical methodologies in accordance with their level of adherence to the principles of green analytical chemistry. Herein, sustainable, sensitive, accurate and cost-effective core-shell molecularly imprinted polymer (MIP) has been developed for the determination of trazodone hydrochloride. It is a widely prescribed medication primarily used to treat depression, anxiety and insomnia. Its detection is significant for ensuring effective therapeutic drug monitoring as it has a narrow therapeutic window in addition to optimize dosages, prevent toxicity, and enhance treatment outcomes. MIP with a uniform core shell structure was prepared where the shell was combined onto the surface of silica nanoparticles by copolymerizing ethylene glycol dimethacrylate together with methacrylic acid in the presence of trazodone hydrochloride. The core consists of silica nanoparticles developed by Stöber method. The core-shell MIP was then embedded as ionophore into the polyvinyl chloride liquid membrane. A linear relationship was found over a dynamic range of 1.0 × 10 <sup>–6</sup> -1.0 × 10 <sup>– 2</sup> M with LOD of 6.0 × 10<sup>–7</sup> M and Nernstian slope of 56.70 mV/decade. The developed method was successfully applied for determination of trazodone hydrochloride in its tablet dosage form with mean percentage recovery of 103.08%. Moreover, the suggested sensor has a significant potential to monitor patients’ plasma level to guarantee drug safety and effectiveness. Additionally, three different approaches namely; Analytical EcoScale, Analytical GREEnness metric approach and finally, the most recent one; Red-Green-Blue model were applied to evaluate the greenness and whiteness profile of the developed method.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"11 ","pages":"Article 100406"},"PeriodicalIF":4.1,"publicationDate":"2025-01-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143159208","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
This work explores the reactivity of sulfur dioxide (SO₂) when adsorbed onto silicon (Si) substitutional doped (8,0) carbon nanotube (Si-CNT) by examining the influence of Si doping on SO₂ adsorption behaviour. Silicon doping maintains the semiconducting nature of pristine carbon nanotubes, with a slight reduction in the band gap from 0.61 eV to 0.54 eV. Moreover, the minimum energy path for SO₂ adsorption on Si-CNTs reveals a chemisorptive process, with an adsorption energy of -1.66 eV, signifying an exothermic reaction where the binding energy of the product exceeds that of the reactants. Molecular orbital analysis supports these findings, showing that the lowest unoccupied molecular orbital (LUMO) is localized on the Si-CNT, while the highest occupied molecular orbital (HOMO) is predominantly located on the SO₂ molecule. Fukui function calculations further show that silicon atom plays a pivotal role by donating electrons to both, the adjacent carbon atoms and the SO₂ molecule. This electron donation leads to a notable accumulation of negative charge on the SO₂ molecule, confirming charge transfer from the Si-CNTs to SO₂. This partial ionic character in the bonding enhances the sensitivity of p-type Si-CNTs to SO₂ molecule.
{"title":"SO2 sensing performance of silicon substitutional doped (8,0) carbon nanotube: A density functional theory study","authors":"Poonam Parkar , Ajay Chaudhari , Mahadev Rangnath Sonawane , Balasaheb Jijaba Nagare","doi":"10.1016/j.talo.2025.100403","DOIUrl":"10.1016/j.talo.2025.100403","url":null,"abstract":"<div><div>This work explores the reactivity of sulfur dioxide (SO₂) when adsorbed onto silicon (Si) substitutional doped (8,0) carbon nanotube (Si-CNT) by examining the influence of Si doping on SO₂ adsorption behaviour. Silicon doping maintains the semiconducting nature of pristine carbon nanotubes, with a slight reduction in the band gap from 0.61 eV to 0.54 eV. Moreover, the minimum energy path for SO₂ adsorption on Si-CNTs reveals a chemisorptive process, with an adsorption energy of -1.66 eV, signifying an exothermic reaction where the binding energy of the product exceeds that of the reactants. Molecular orbital analysis supports these findings, showing that the lowest unoccupied molecular orbital (LUMO) is localized on the Si-CNT, while the highest occupied molecular orbital (HOMO) is predominantly located on the SO₂ molecule. Fukui function calculations further show that silicon atom plays a pivotal role by donating electrons to both, the adjacent carbon atoms and the SO₂ molecule. This electron donation leads to a notable accumulation of negative charge on the SO₂ molecule, confirming charge transfer from the Si-CNTs to SO₂. This partial ionic character in the bonding enhances the sensitivity of p-type Si-CNTs to SO₂ molecule.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"11 ","pages":"Article 100403"},"PeriodicalIF":4.1,"publicationDate":"2025-01-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143159136","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-01-10DOI: 10.1016/j.talo.2025.100404
Azza H. Rageh , Mohamed I. Said , Asmaa Abdeltawab , Fatma A.M. Abdel-aal
This study uniquely emphasizes the crucial role of MOF synthesis techniques in optimizing electrocatalytic properties and enhancing electroanalytical performance. The main aim of this work is to develop a highly sensitive, selective, and cost-effective electrochemical sensor for detecting sunitinib malate (SUN) in serum samples collected from renal cancer patients. The designed sensor was based on using CuO nanoparticles/lanthanum 1,4-napthalene dicarboxylic acid (NDC) MOF-modified carbon paste electrode (CuO NPs/LaNDC-MOF/CPE) coupled with square-wave adsorptive anodic stripping voltammetry (SW-AdASV) as the electrochemical technique. Two MOF synthetic approaches were utilized i.e. conventional (Conv.) and solvothermal (Solvo.). The synthesized La-MOFs were characterized using X-ray Diffraction analysis (XRD), Fourier transform IR spectroscopy (FTIR), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM) and Nitrogen adsorption/desorption isotherm (BET). LaNDC-MOF (Conv.) has a higher surface area (four times) than LaNDC-MOF (Solvo.). Moreover, the modified electrode based on LaNDC-MOF (Conv.) exhibited better electrocatalytic activity and improved sensitivity towards the oxidation of SUN than that prepared through solvothermal route. Various experimental parameters, including accumulation potential, accumulation time, and pH of the supporting electrolyte, were optimized to obtain the best analytical performance. The fabricated sensor based on CuO NPs/LaNDC-MOF/CPE showed an oxidation peak of SUN at 0.66 V vs Ag/AgCl. Under the optimized conditions, SW-AdASV method exhibited a linear response over a concentration range of 0.01–1.0 μmol l-1 with a detection limit of 0.002 μmol l-1 for SUN. The proposed method was successfully applied for the determination of SUN in pharmaceutical formulations and serum samples of renal cancer patients. Moreover, the proposed methodology via modification of CPE with the synthesized MOFs tailors them to be applied for clinical analysis and therapeutic drug monitoring of SUN, providing a valuable tool for personalized medicine and improving the treatment outcomes for renal cancer patients.
{"title":"Innovative MOF-enhanced electroanalytical approach for sensitive sunitinib malate detection in renal carcinoma patients using CuO/lanthanum MOF-modified carbon paste electrode","authors":"Azza H. Rageh , Mohamed I. Said , Asmaa Abdeltawab , Fatma A.M. Abdel-aal","doi":"10.1016/j.talo.2025.100404","DOIUrl":"10.1016/j.talo.2025.100404","url":null,"abstract":"<div><div>This study uniquely emphasizes the crucial role of MOF synthesis techniques in optimizing electrocatalytic properties and enhancing electroanalytical performance. The main aim of this work is to develop a highly sensitive, selective, and cost-effective electrochemical sensor for detecting sunitinib malate (SUN) in serum samples collected from renal cancer patients. The designed sensor was based on using CuO nanoparticles/lanthanum 1,4-napthalene dicarboxylic acid (NDC) MOF-modified carbon paste electrode (CuO NPs/LaNDC-MOF/CPE) coupled with square-wave adsorptive anodic stripping voltammetry (SW-AdASV) as the electrochemical technique. Two MOF synthetic approaches were utilized i.e. conventional (Conv.) and solvothermal (Solvo.). The synthesized La-MOFs were characterized using X-ray Diffraction analysis (XRD), Fourier transform IR spectroscopy (FTIR), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM) and Nitrogen adsorption/desorption isotherm (BET). LaNDC-MOF (Conv.) has a higher surface area (four times) than LaNDC-MOF (Solvo.). Moreover, the modified electrode based on LaNDC-MOF (Conv.) exhibited better electrocatalytic activity and improved sensitivity towards the oxidation of SUN than that prepared through solvothermal route. Various experimental parameters, including accumulation potential, accumulation time, and pH of the supporting electrolyte, were optimized to obtain the best analytical performance. The fabricated sensor based on CuO NPs/LaNDC-MOF/CPE showed an oxidation peak of SUN at 0.66 V vs Ag/AgCl. Under the optimized conditions, SW-AdASV method exhibited a linear response over a concentration range of 0.01–1.0 μmol <span>l</span><sup>-1</sup> with a detection limit of 0.002 μmol <span>l</span><sup>-1</sup> for SUN. The proposed method was successfully applied for the determination of SUN in pharmaceutical formulations and serum samples of renal cancer patients. Moreover, the proposed methodology via modification of CPE with the synthesized MOFs tailors them to be applied for clinical analysis and therapeutic drug monitoring of SUN, providing a valuable tool for personalized medicine and improving the treatment outcomes for renal cancer patients.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"11 ","pages":"Article 100404"},"PeriodicalIF":4.1,"publicationDate":"2025-01-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143159139","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-01-09DOI: 10.1016/j.talo.2025.100402
Ruchika Thayil, Saidi Reddy Parne
Nanomaterials, known for their unique chemical and physical properties at the nanoscale, are crucial in advancing various cutting-edge applications. The distinct size-dependent behaviors and surface characteristics set them apart. Among these materials, molybdenum disulfide (MoS2) has gained considerable interest for room-temperature gas detection due to its high surface area, improved reactivity from the surface, and excellent carrier mobility, which makes it effective in sensing applications. In this work, MoS2 with excess sodium molybdate dihydrate (MoS2(Mo)) and MoS2 with excess thioacetamide (MoS2(S)) were synthesized using the hydrothermal method and tested for toluene gas sensing at various concentrations. The results indicate that MoS2(S) showed ΔR/Rair% of 343 % compared to MoS2(Mo), which is 197 % for 20 ppm toluene gas. In addition, MoS2(S) showed reduced response/recovery time. The results suggest that these MoS2-based sensors can be used for the development of room temperature sensors for toluene sensing.
{"title":"Tuning MoS2 nanostructures for superior room-temperature toluene sensing","authors":"Ruchika Thayil, Saidi Reddy Parne","doi":"10.1016/j.talo.2025.100402","DOIUrl":"10.1016/j.talo.2025.100402","url":null,"abstract":"<div><div>Nanomaterials, known for their unique chemical and physical properties at the nanoscale, are crucial in advancing various cutting-edge applications. The distinct size-dependent behaviors and surface characteristics set them apart. Among these materials, molybdenum disulfide (MoS<sub>2</sub>) has gained considerable interest for room-temperature gas detection due to its high surface area, improved reactivity from the surface, and excellent carrier mobility, which makes it effective in sensing applications. In this work, MoS<sub>2</sub> with excess sodium molybdate dihydrate (MoS<sub>2</sub>(Mo)) and MoS<sub>2</sub> with excess thioacetamide (MoS<sub>2</sub>(S)) were synthesized using the hydrothermal method and tested for toluene gas sensing at various concentrations. The results indicate that MoS<sub>2</sub>(S) showed ΔR/R<sub>air</sub>% of 343 % compared to MoS<sub>2</sub>(Mo), which is 197 % for 20 ppm toluene gas. In addition, MoS<sub>2</sub>(S) showed reduced response/recovery time. The results suggest that these MoS<sub>2</sub>-based sensors can be used for the development of room temperature sensors for toluene sensing.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"11 ","pages":"Article 100402"},"PeriodicalIF":4.1,"publicationDate":"2025-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143159155","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-01-07DOI: 10.1016/j.talo.2025.100401
Momen Sahriar Shoshi , Md Abu Huraiya , Vinoth Raj R , Abror Jawad , Chang Yi Kong , Hitoshi Tabata , Sankar Ganesh Ramaraj , S.M. Abdur Razzak
This study represents a new design for an empathetic surface plasmon resonance (SPR) sensor that utilizes BlueP/TMDCs and BaTiO3 (barium titanate) and employs the angular interrogation technique to measure the glucose concentration level in urine samples. This design optimization involved extensive numerical analysis through the use of the Transfer Matrix Method (TMM) at a visible wavelength of λ=633 nm to enhance sensitivity, full width half maximum (FWHM), detection accuracy (DA), and quality factor (QF). Additionally, Finite Element Method (FEM) analysis was used to ensure the accuracy of the findings achieved through Transfer Matrix Method (TMM). The suggested biosensor configuration involves five layers: a BK-7 glass prism, 56 nm Ag layer, 11 nm BaTiO3 layer, BlueP/TMDCs with thickness of 0.68 nm, and a sensing medium (urine sample). Unlike earlier designs relying on conventional 2D materials or single dielectric layers, the proposed hybrid structure not only enhances light-matter interaction and optimizes electromagnetic field distribution but also outperforms other hybrid sensors by achieving superior sensitivity, detection accuracy, and quality factor. Through the use of novel combination of BlueP/TMDCs and BaTiO₃ in this hybrid sensor, the biosensor achieved significantly improved performance, with enhanced sensitivity of 435 deg/RIU at a concentration of glucose 10 g/dL, QF of 86.29442 RIU−1 as well as DA of 0.190114 deg−1 spanning a refractive index (RI) from 1.335 to 1.347.
{"title":"Revolutionary barium titanate-BlueP/TMDCs SPR sensor: Ultra-sensitive detection of urine glucose levels","authors":"Momen Sahriar Shoshi , Md Abu Huraiya , Vinoth Raj R , Abror Jawad , Chang Yi Kong , Hitoshi Tabata , Sankar Ganesh Ramaraj , S.M. Abdur Razzak","doi":"10.1016/j.talo.2025.100401","DOIUrl":"10.1016/j.talo.2025.100401","url":null,"abstract":"<div><div>This study represents a new design for an empathetic surface plasmon resonance (SPR) sensor that utilizes BlueP/TMDCs and BaTiO<sub>3</sub> (barium titanate) and employs the angular interrogation technique to measure the glucose concentration level in urine samples. This design optimization involved extensive numerical analysis through the use of the Transfer Matrix Method (TMM) at a visible wavelength of λ=633 nm to enhance sensitivity, full width half maximum (FWHM), detection accuracy (DA), and quality factor (QF). Additionally, Finite Element Method (FEM) analysis was used to ensure the accuracy of the findings achieved through Transfer Matrix Method (TMM). The suggested biosensor configuration involves five layers: a BK-7 glass prism, 56 nm Ag layer, 11 nm BaTiO<sub>3</sub> layer, BlueP/TMDCs with thickness of 0.68 nm, and a sensing medium (urine sample). Unlike earlier designs relying on conventional 2D materials or single dielectric layers, the proposed hybrid structure not only enhances light-matter interaction and optimizes electromagnetic field distribution but also outperforms other hybrid sensors by achieving superior sensitivity, detection accuracy, and quality factor. Through the use of novel combination of BlueP/TMDCs and BaTiO₃ in this hybrid sensor, the biosensor achieved significantly improved performance, with enhanced sensitivity of 435 deg/RIU at a concentration of glucose 10 g/dL, QF of 86.29442 RIU<sup>−1</sup> as well as DA of 0.190114 deg<sup>−1</sup> spanning a refractive index (RI) from 1.335 to 1.347.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"11 ","pages":"Article 100401"},"PeriodicalIF":4.1,"publicationDate":"2025-01-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143159156","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-01-04DOI: 10.1016/j.talo.2025.100400
Ting Liang , Min Luo , Ling Shi , Hongping Yang , Guangming Yang
In this work, a nanocomposite of molybdenum disulfide (MoS₂) and graphene (r-GO) was synthesized using hydrothermal method, and was subsequently employed as a dopant to fabricate a hybrid coating of polypyrrole (PPy)-r-GO-MoS₂ via cyclic voltammetry (CV). The resulting coating was applied to extract five phenolic compounds, and combined with gas chromatography-mass spectrometry (GC–MS) to establish an analytical method for the determination of 3‑chloro-4-fluorophenol, 2‑chloro-4-methoxyphenol, 2,6-dimethoxyphenol, 2,4,6-trichlorophenol, and 2,6-dichloro-4-nitrophenol in environmental samples. The results indicated that PPy-MoS₂-r-GO coating exhibited superior extraction efficiency in comparison with to PPy coating. To optimize testing conditions, MoS₂-r-GO concentration for the electrochemical preparation of the coating, extraction conditions, including time, temperature, and stirring speed, were also investigated. Consequently, the analytical method exhibited an excellent linear response, with a correlation coefficient ranging from 0.9950 to 0.9980 for the five phenolic compounds in the range of 0.01 μg L⁻¹ to 50 μg L⁻¹. The detection limits were 0.00550 μg L⁻¹ - 0.00850 μg L⁻¹. This method was employed to detect phenol in real samples, yielding recoveries ranging from 89.60 % to 103.30 %, thereby confirming its practical applicability.
{"title":"Electrochemical preparation of polypyrrole-molybdenum disulfide-graphene nanocomposite coating for the determination of phenols","authors":"Ting Liang , Min Luo , Ling Shi , Hongping Yang , Guangming Yang","doi":"10.1016/j.talo.2025.100400","DOIUrl":"10.1016/j.talo.2025.100400","url":null,"abstract":"<div><div>In this work, a nanocomposite of molybdenum disulfide (MoS₂) and graphene (r-GO) was synthesized using hydrothermal method, and was subsequently employed as a dopant to fabricate a hybrid coating of polypyrrole (PPy)-r-GO-MoS₂ via cyclic voltammetry (CV). The resulting coating was applied to extract five phenolic compounds, and combined with gas chromatography-mass spectrometry (GC–MS) to establish an analytical method for the determination of 3‑chloro-4-fluorophenol, 2‑chloro-4-methoxyphenol, 2,6-dimethoxyphenol, 2,4,6-trichlorophenol, and 2,6-dichloro-4-nitrophenol in environmental samples. The results indicated that PPy-MoS₂-r-GO coating exhibited superior extraction efficiency in comparison with to PPy coating. To optimize testing conditions, MoS₂-r-GO concentration for the electrochemical preparation of the coating, extraction conditions, including time, temperature, and stirring speed, were also investigated. Consequently, the analytical method exhibited an excellent linear response, with a correlation coefficient ranging from 0.9950 to 0.9980 for the five phenolic compounds in the range of 0.01 μg L⁻¹ to 50 μg L⁻¹. The detection limits were 0.00550 μg L⁻¹ - 0.00850 μg L⁻¹. This method was employed to detect phenol in real samples, yielding recoveries ranging from 89.60 % to 103.30 %, thereby confirming its practical applicability.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"11 ","pages":"Article 100400"},"PeriodicalIF":4.1,"publicationDate":"2025-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143159214","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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