Pub Date : 2025-08-15DOI: 10.1016/j.talo.2025.100531
Xue Li , Zijiao Zhang , Tian Tian , Chen Chen , Xin Xu , Yuzhu He , Yaran Zang , Jianan Hui , Hongju Mao , Huiying Liu
Bone organoids hold great promise for modeling bone-related diseases, improving bone injury repair strategies, and enabling high-throughput drug screening. However, conventional approaches rely heavily on matrix biomaterials—such as Matrigel, collagen gels, or 3D-printed scaffolds—which introduce undefined parameters, pose manufacturing complexities, and raise cost barriers, potentially limiting clinical translation. To address these challenges, we present a novel high-throughput microfluidic chip that generates 540 uniformly sized, scaffold-free 3D bone organoids simultaneously within six independent channels. By co-cultivating human bone marrow mesenchymal stem cells (hBMSCs), human umbilical vein endothelial cells (HUVECs), and mineralized collagen (MC), self-assembled bone organoids formed by the third day and progressively compacted over time, exhibiting enhanced cell viability and proliferation. The inclusion of MC upregulated multiple osteogenic markers (OCN, ALP, COL-1, RUNX2, and BMP-2), while endothelial markers (PECAM-1, HIF-1α, and VEGF) remained consistently expressed, reflecting stable vascularization and mineralization potential. Overall, this high-throughput, matrix-free microfluidic platform offers a biomimetic environment for the investigation of osteogenesis and angiogenesis and holds significant promise for advanced material assessment, drug screening, and disease modeling.
{"title":"High-throughput microfluidic generation of self-assembled, uniform 3D vascularized and mineralized bone organoids without matrix biomaterials","authors":"Xue Li , Zijiao Zhang , Tian Tian , Chen Chen , Xin Xu , Yuzhu He , Yaran Zang , Jianan Hui , Hongju Mao , Huiying Liu","doi":"10.1016/j.talo.2025.100531","DOIUrl":"10.1016/j.talo.2025.100531","url":null,"abstract":"<div><div>Bone organoids hold great promise for modeling bone-related diseases, improving bone injury repair strategies, and enabling high-throughput drug screening. However, conventional approaches rely heavily on matrix biomaterials—such as Matrigel, collagen gels, or 3D-printed scaffolds—which introduce undefined parameters, pose manufacturing complexities, and raise cost barriers, potentially limiting clinical translation. To address these challenges, we present a novel high-throughput microfluidic chip that generates 540 uniformly sized, scaffold-free 3D bone organoids simultaneously within six independent channels. By co-cultivating human bone marrow mesenchymal stem cells (hBMSCs), human umbilical vein endothelial cells (HUVECs), and mineralized collagen (MC), self-assembled bone organoids formed by the third day and progressively compacted over time, exhibiting enhanced cell viability and proliferation. The inclusion of MC upregulated multiple osteogenic markers (OCN, ALP, COL-1, RUNX2, and BMP-2), while endothelial markers (PECAM-1, HIF-1α, and VEGF) remained consistently expressed, reflecting stable vascularization and mineralization potential. Overall, this high-throughput, matrix-free microfluidic platform offers a biomimetic environment for the investigation of osteogenesis and angiogenesis and holds significant promise for advanced material assessment, drug screening, and disease modeling.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"12 ","pages":"Article 100531"},"PeriodicalIF":3.7,"publicationDate":"2025-08-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144904572","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-08-12DOI: 10.1016/j.talo.2025.100529
Ankita Ghosh , Ramesh Chandra , Nidhi Chauhan
Beta-endorphin (BE) is an endogenous opioid peptide (EOP) produced in the anterior pituitary gland and hypothalamus. Beta-endorphin is a vital neurotransmitter involved in physiological processes including relief the pain, boosting memory, and regulating mood. BE is a happy hormone that reduces the chance of depression and anxiety. BE analysed by traditional laboratory techniques like LC-MS, ELISA and radioimmunoassay is reliable; however, there are certain limitations including time consumption, device complexity, cost and availability. This study aims to develop a self-monitoring molecularly imprinted polymer-based (MIP) biosensor for sensitive, selective and rapid detection of BE. The nanocomposite TiO2/MoS2 was electrochemically deposited on the screen-printed electrode using cyclic voltammetry (CV) to enhance the conductivity and surface area to immobilize MIP. The MIP was electrochemically deposited at voltage range 0.2 to -0.6 V using CV for 20 cycles at scan rate 50 mV/s on the modified TiO2/MoS2/SPE. MIP is a synthetic bio-recognizing element that provides high selectivity for BE over other structurally similar molecules. The developed sensor MIP@TiO2/MoS2/SPE exhibits sensitivity of 0.475 µA/pM, the limit of detection (LOD) of 0.1pM and a detection range of 0.1pM and 200pM. This is novel, innovative and cost-effective point of care device developed for the rapid and real time detection of BE.
{"title":"Chemical imprinting meets nanotechnology: Ultra-sensitive monitoring of beta-endorphin","authors":"Ankita Ghosh , Ramesh Chandra , Nidhi Chauhan","doi":"10.1016/j.talo.2025.100529","DOIUrl":"10.1016/j.talo.2025.100529","url":null,"abstract":"<div><div>Beta-endorphin (BE) is an endogenous opioid peptide (EOP) produced in the anterior pituitary gland and hypothalamus. Beta-endorphin is a vital neurotransmitter involved in physiological processes including relief the pain, boosting memory, and regulating mood. BE is a happy hormone that reduces the chance of depression and anxiety. BE analysed by traditional laboratory techniques like LC-MS, ELISA and radioimmunoassay is reliable; however, there are certain limitations including time consumption, device complexity, cost and availability. This study aims to develop a self-monitoring molecularly imprinted polymer-based (MIP) biosensor for sensitive, selective and rapid detection of BE. The nanocomposite TiO<sub>2</sub>/MoS<sub>2</sub> was electrochemically deposited on the screen-printed electrode using cyclic voltammetry (CV) to enhance the conductivity and surface area to immobilize MIP. The MIP was electrochemically deposited at voltage range 0.2 to -0.6 V using CV for 20 cycles at scan rate 50 mV/s on the modified TiO<sub>2</sub>/MoS<sub>2</sub>/SPE. MIP is a synthetic bio-recognizing element that provides high selectivity for BE over other structurally similar molecules. The developed sensor MIP@TiO<sub>2</sub>/MoS<sub>2</sub>/SPE exhibits sensitivity of 0.475 µA/pM, the limit of detection (LOD) of 0.1pM and a detection range of 0.1pM and 200pM. This is novel, innovative and cost-effective point of care device developed for the rapid and real time detection of BE.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"12 ","pages":"Article 100529"},"PeriodicalIF":3.7,"publicationDate":"2025-08-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144887024","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Dispersive Liquid–Liquid Microextraction (DLLME) has evolved significantly by integrating physical assistance methods to enhance extraction efficiency while minimizing the use of organic solvents and disperser agents. This review critically examines the latest advancements in assisted DLLME techniques, including ultrasound-assisted DLLME, vortex-assisted DLLME, and air-assisted DLLME methods, with an emphasis on their potential to minimize or eliminate the use of toxic organic solvents and disperser agents. These environmentally friendly approaches are particularly important for detecting hazardous contaminants such as organophosphorus pesticides (OPPs), which are widely used in agriculture and known for their acute neurotoxicity, environmental persistence, and potential to disrupt nervous systems. OPPs can cause severe neurological effects even at trace levels. Their continued presence in food, water, and environmental samples underscores the urgent need for highly sensitive and reliable detection methods to ensure public safety and regulatory compliance. The review highlights how greener DLLME techniques contribute to sustainable analytical practices by reducing or eliminating harmful chemicals. Comparative evaluations are presented for enrichment factors, extraction times, and analyte recoveries across various sample types, including environmental water, biological fluids, and food products. Finally, the review discusses future directions toward achieving completely solvent-free and disperser-free DLLME systems through innovative hybrid and energy-assisted strategies.
{"title":"Solvent extraction methods towards efficient recognition of organophosphorus pesticides: Recent progress and analytical challenges","authors":"Marzieh Fallahi Nezhad , Amin Foroozandeh , Hossein Salar Amoli , Mohammad Hasanzadeh","doi":"10.1016/j.talo.2025.100530","DOIUrl":"10.1016/j.talo.2025.100530","url":null,"abstract":"<div><div>Dispersive Liquid–Liquid Microextraction (DLLME) has evolved significantly by integrating physical assistance methods to enhance extraction efficiency while minimizing the use of organic solvents and disperser agents. This review critically examines the latest advancements in assisted DLLME techniques, including ultrasound-assisted DLLME, vortex-assisted DLLME, and air-assisted DLLME methods, with an emphasis on their potential to minimize or eliminate the use of toxic organic solvents and disperser agents. These environmentally friendly approaches are particularly important for detecting hazardous contaminants such as organophosphorus pesticides (OPPs), which are widely used in agriculture and known for their acute neurotoxicity, environmental persistence, and potential to disrupt nervous systems. OPPs can cause severe neurological effects even at trace levels. Their continued presence in food, water, and environmental samples underscores the urgent need for highly sensitive and reliable detection methods to ensure public safety and regulatory compliance. The review highlights how greener DLLME techniques contribute to sustainable analytical practices by reducing or eliminating harmful chemicals. Comparative evaluations are presented for enrichment factors, extraction times, and analyte recoveries across various sample types, including environmental water, biological fluids, and food products. Finally, the review discusses future directions toward achieving completely solvent-free and disperser-free DLLME systems through innovative hybrid and energy-assisted strategies.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"12 ","pages":"Article 100530"},"PeriodicalIF":3.7,"publicationDate":"2025-08-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144865128","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-08-06DOI: 10.1016/j.talo.2025.100525
Ivana Tomac , Veronika Mikušová , Peter Mikuš , Jan Labuda
Numerous analytical methods were developed based on purely chemical, electrochemical and other physicochemical (spectral, chromatographic) interactions of the antioxidants (AOx) molecules with corresponding specific thermodynamic and kinetic background of experimental, mostly in vitro, conditions. Highly useful results are widely available which are however, operationally based and, therefore, not simply comparable. Reflecting the role of AOx in living organisms characterized by the biomolecular interactions, analytical procedures are also developed based on the antioxidant – pro-oxidant interactions in the presence of a biomolecule. In this case, enzymes fulfil the role of probe expressing an inhibition of their catalytic activity or nucleic acids, lipids, and others are the targets competing with AOx at a pro-oxidant attack. This review presents recent approaches and results on the analytical utilization of inhibiting and competing interactions with AOx. Novel trends exploiting nanomaterials and nanozymes are included. The studies of plant-derived extracts and products are particularly treated being of high pharmaceutical and medical interests. General features with future challenges regarding methods standardization development of portable devices and miniaturization technologies are highlighted to stimulate further progress in the effective AOx detection and characterization.
{"title":"Effective detection of antioxidants using functional schemes of enzyme inhibition and competing (bio)reactions","authors":"Ivana Tomac , Veronika Mikušová , Peter Mikuš , Jan Labuda","doi":"10.1016/j.talo.2025.100525","DOIUrl":"10.1016/j.talo.2025.100525","url":null,"abstract":"<div><div>Numerous analytical methods were developed based on purely chemical, electrochemical and other physicochemical (spectral, chromatographic) interactions of the antioxidants (AOx) molecules with corresponding specific thermodynamic and kinetic background of experimental, mostly <em>in vitro</em>, conditions. Highly useful results are widely available which are however, operationally based and, therefore, not simply comparable. Reflecting the role of AOx in living organisms characterized by the biomolecular interactions, analytical procedures are also developed based on the antioxidant – pro-oxidant interactions in the presence of a biomolecule. In this case, enzymes fulfil the role of probe expressing an inhibition of their catalytic activity or nucleic acids, lipids, and others are the targets competing with AOx at a pro-oxidant attack. This review presents recent approaches and results on the analytical utilization of inhibiting and competing interactions with AOx. Novel trends exploiting nanomaterials and nanozymes are included. The studies of plant-derived extracts and products are particularly treated being of high pharmaceutical and medical interests. General features with future challenges regarding methods standardization development of portable devices and miniaturization technologies are highlighted to stimulate further progress in the effective AOx detection and characterization.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"12 ","pages":"Article 100525"},"PeriodicalIF":3.7,"publicationDate":"2025-08-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144841970","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Oroxylum indicum (L.) Kurz (OI) or Shyonaka or Sona Patha is an endangered medicinal plant used in various traditional medicines. The roots of OI are the most commonly used part in preparing numerous traditional medicines worldwide. To conserve the environment, it is necessary to check the substitution of official parts with aerial parts like leaf and stem bark using sophisticated techniques. The present study developed HPLC and ICP-OES methods to quantify OI's main phytoconstituents and metal ions in four parts (root, root bark, stem bark, and leaf). The phytochemicals viz. vanillic acid, trans-ferulic acid, baicalein, and chrysin were quantified by HPLC study, where the significantly better amounts of baicalein and chrysin (baicalein > chrysin) were quantified in aerial parts (leaf and stem bark) as compared to root and root bark. ICP-OES elemental analysis has revealed that all parts of OI are good sources of Ca, K, Na, Mg, Mn, Fe, and Zn. GC–MS study was performed to identify the volatile compounds of all parts of OI. In antioxidant studies (TPC, TFC, and DPPH assays), the leaf showed a better IC50 value, followed by stem bark, root bark, and root. In the antacid study, the leaf has shown better activity, followed by root bark, stem bark, and root. In the anti-bacterial assay, all parts of OI significantly inhibited Staphylococcus aureus and Salmonella typhi strains, where root bark and leaf demonstrated improved activities. In computational studies, the invitro antacid, antioxidant, and anti-bacterial activities were confirmed, where most of the phytochemicals demonstrated binding energies over standard drugs. Overall, the study revealed that all parts of OI, including roots and aerial parts, might be medicinally useful, and leaves may be used as a nutritional food. Moreover, the official part, i.e., root or root bark used in traditional medicines, may be replaced with aerial parts (leaf or stem bark) to conserve the environment. After the in-depth pharmacological and toxicological studies, all parts of OI Oroxylum indicum might be incorporated into pharmaceutics.
{"title":"Quantification of phytochemicals of different parts of Oroxylum indicum (L.) Kurz for the evidence-based substitution of the official part (root) with aerial part","authors":"Megha Nigam , Yashika Gandhi , Vijay Kumar , Hemant Soni , Rishi Kumar Saxena","doi":"10.1016/j.talo.2025.100528","DOIUrl":"10.1016/j.talo.2025.100528","url":null,"abstract":"<div><div><em>Oroxylum indicum</em> (L.) Kurz (OI) or Shyonaka or Sona Patha is an endangered medicinal plant used in various traditional medicines. The roots of OI are the most commonly used part in preparing numerous traditional medicines worldwide. To conserve the environment, it is necessary to check the substitution of official parts with aerial parts like leaf and stem bark using sophisticated techniques. The present study developed HPLC and ICP-OES methods to quantify OI's main phytoconstituents and metal ions in four parts (root, root bark, stem bark, and leaf). The phytochemicals viz. vanillic acid, trans-ferulic acid, baicalein, and chrysin were quantified by HPLC study, where the significantly better amounts of baicalein and chrysin (baicalein > chrysin) were quantified in aerial parts (leaf and stem bark) as compared to root and root bark. ICP-OES elemental analysis has revealed that all parts of OI are good sources of Ca, K, Na, Mg, Mn, Fe, and Zn. GC–MS study was performed to identify the volatile compounds of all parts of OI. In antioxidant studies (TPC, TFC, and DPPH assays), the leaf showed a better IC<sub>50</sub> value, followed by stem bark, root bark, and root. In the antacid study, the leaf has shown better activity, followed by root bark, stem bark, and root. In the anti-bacterial assay, all parts of OI significantly inhibited <em>Staphylococcus aureus</em> and <em>Salmonella typhi</em> strains, where root bark and leaf demonstrated improved activities. In computational studies, the invitro antacid, antioxidant, and anti-bacterial activities were confirmed, where most of the phytochemicals demonstrated binding energies over standard drugs. Overall, the study revealed that all parts of OI, including roots and aerial parts, might be medicinally useful, and leaves may be used as a nutritional food. Moreover, the official part, i.e., root or root bark used in traditional medicines, may be replaced with aerial parts (leaf or stem bark) to conserve the environment. After the in-depth pharmacological and toxicological studies, all parts of OI <em>Oroxylum indicum</em> might be incorporated into pharmaceutics.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"12 ","pages":"Article 100528"},"PeriodicalIF":3.7,"publicationDate":"2025-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144830544","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-08-05DOI: 10.1016/j.talo.2025.100527
Peng Liu , Sitian He , Mette Ø. Agerbæk , Ali Salanti , Leon W.M.M. Terstappen , Pascal Jonkheijm , Michiel Stevens
Introduction
The transcriptomic analysis of circulating tumor cells provides valuable insights into cancer metastasis, heterogeneity and the identification of drugable targets. However, traditional methods for circulating tumor cel identification and isolation often compromise mRNA integrity, due to cell handling such as the cell permeabilization, required for intracellular staining. Here, we present a novel identification and isolation pipeline for single cell transcriptomics of magnetically enriched tumor by combining rVAR2 based identification cells with single-cell magnetic pickup.
Methods
To test our method, we used tumor cells from four lung cancer cell lines spiked into blood. After magnetic enrichment using the CellSearch® Profile Kit, the resulting sample was divided for staining with either rVAR2 or CellSearch reagents. Single cells were isolated using a magnetic needle and analyzed for mRNA integrity using reverse transcription quantitative polymerase chain reaction (RT-qPCR) targeting the GAPDH and EpCAM genes.
Results
The integration of single-cell magnetic pickup enabled precise single-cell separation, while the extracellular rVAR2 staining enables mRNA preservation, collectively facilitating the detection of low-expressed genes at the single-cell level. Compared to CellSearch staining, the rVAR2 staining resulted in our pipeline in a approximately 10 to 100 times higher mRNA yield from single magnetically enriched tumor cells.
Conclusion
This mRNA-friendly method enhances our ability to study tumor heterogeneity at the single-cell level and supports the development of personalized cancer therapies, making it a valuable tool for circulating tumor cel research and clinical applications.
{"title":"Identification and isolation pipeline for single cell transcriptomic of magnetically enriched tumor cells","authors":"Peng Liu , Sitian He , Mette Ø. Agerbæk , Ali Salanti , Leon W.M.M. Terstappen , Pascal Jonkheijm , Michiel Stevens","doi":"10.1016/j.talo.2025.100527","DOIUrl":"10.1016/j.talo.2025.100527","url":null,"abstract":"<div><h3>Introduction</h3><div>The transcriptomic analysis of circulating tumor cells provides valuable insights into cancer metastasis, heterogeneity and the identification of drugable targets. However, traditional methods for circulating tumor cel identification and isolation often compromise mRNA integrity, due to cell handling such as the cell permeabilization, required for intracellular staining. Here, we present a novel identification and isolation pipeline for single cell transcriptomics of magnetically enriched tumor by combining rVAR2 based identification cells with single-cell magnetic pickup.</div></div><div><h3>Methods</h3><div>To test our method, we used tumor cells from four lung cancer cell lines spiked into blood. After magnetic enrichment using the CellSearch® Profile Kit, the resulting sample was divided for staining with either rVAR2 or CellSearch reagents. Single cells were isolated using a magnetic needle and analyzed for mRNA integrity using reverse transcription quantitative polymerase chain reaction (RT-qPCR) targeting the GAPDH and EpCAM genes.</div></div><div><h3>Results</h3><div>The integration of single-cell magnetic pickup enabled precise single-cell separation, while the extracellular rVAR2 staining enables mRNA preservation, collectively facilitating the detection of low-expressed genes at the single-cell level. Compared to CellSearch staining, the rVAR2 staining resulted in our pipeline in a approximately 10 to 100 times higher mRNA yield from single magnetically enriched tumor cells.</div></div><div><h3>Conclusion</h3><div>This mRNA-friendly method enhances our ability to study tumor heterogeneity at the single-cell level and supports the development of personalized cancer therapies, making it a valuable tool for circulating tumor cel research and clinical applications.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"12 ","pages":"Article 100527"},"PeriodicalIF":3.7,"publicationDate":"2025-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144830522","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-07-19DOI: 10.1016/j.talo.2025.100520
Manohar S K , Gowrav M P , Mounika P , Karthika Paul , Hemanth Vikram P R , Maged Mohammed Abdo Mohsen , Bannimath Gurupadayya
Introduction
Residual solvents like dimethyl sulfoxide (DMSO), commonly used in the formulation of paliperidone nanocrystals, require stringent quantification to ensure safety and regulatory compliance. This study presents the development of a novel, sensitive, and specific Gas Chromatography-Flame Ionization Detector (GC-FID) method for their accurate determination.
Methodology
Paliperidone nanocrystals were prepared by the antisolvent precipitation method. A novel analytical method was developed by using gas chromatography for residual solvent analysis present in nanocrystals. The analytical method utilized an Rtx column (dimensions: 30.0 mm x 0.25 mm) with nitrogen gas as the carrier and methanol as the diluent. The developed gas chromatography method was validated as per ICH Q2 (R1) guidelines.
Results
Analysis via GC-FID yielded a prominent peak for the residual solvent, dimethyl sulfoxide (DMSO), at a retention time of 1.819 minutes under a pressure of 170.3 kPa and a flow rate of 28 mL/min. The GC oven temperature commenced at 50 °C and was maintained for 3 minutes. Subsequently, a programmed ramp of 10 °C/minute was applied until a final temperature of 100 °C was reached, which was then held for 3 minutes. The detector temperature was constant at 250 °C. Validation following ICH guidelines confirmed method specificity, sensitivity and linearity within a 2–10 µL/mL range. The Limit of Detection (LOD) and Limit of Quantification (LOQ) were found to be 0.0047 µL/mL and 0.0136 µL/mL, respectively. The residual solvent DMSO in the 1 mg of paliperidone nanocrystal sample was found to be 21.91 ppm. Greenness and whiteness evaluation were performed for the developed method.
Conclusion
This novel GC-FID method offers a robust and dependable analytical approach for the determination of residual solvents in paliperidone nanocrystals and has an application in the routine quality control analysis. Moreover, the method aligns with green analytical chemistry principles by incorporating low solvent consumption, reduced waste generation, and energy-efficient operation, thereby supporting environmentally sustainable pharmaceutical quality control.
{"title":"Development of a green GC-FID method for residual solvent analysis in paliperidone nanocrystal formulations: Validation and greenness assessment","authors":"Manohar S K , Gowrav M P , Mounika P , Karthika Paul , Hemanth Vikram P R , Maged Mohammed Abdo Mohsen , Bannimath Gurupadayya","doi":"10.1016/j.talo.2025.100520","DOIUrl":"10.1016/j.talo.2025.100520","url":null,"abstract":"<div><h3>Introduction</h3><div>Residual solvents like dimethyl sulfoxide (DMSO), commonly used in the formulation of paliperidone nanocrystals, require stringent quantification to ensure safety and regulatory compliance. This study presents the development of a novel, sensitive, and specific Gas Chromatography-Flame Ionization Detector (GC-FID) method for their accurate determination.</div></div><div><h3>Methodology</h3><div>Paliperidone nanocrystals were prepared by the antisolvent precipitation method. A novel analytical method was developed by using gas chromatography for residual solvent analysis present in nanocrystals. The analytical method utilized an Rtx column (dimensions: 30.0 mm x 0.25 mm) with nitrogen gas as the carrier and methanol as the diluent. The developed gas chromatography method was validated as per ICH Q2 (R1) guidelines.</div></div><div><h3>Results</h3><div>Analysis via GC-FID yielded a prominent peak for the residual solvent, dimethyl sulfoxide (DMSO), at a retention time of 1.819 minutes under a pressure of 170.3 kPa and a flow rate of 28 mL/min. The GC oven temperature commenced at 50 °C and was maintained for 3 minutes. Subsequently, a programmed ramp of 10 °C/minute was applied until a final temperature of 100 °C was reached, which was then held for 3 minutes. The detector temperature was constant at 250 °C. Validation following ICH guidelines confirmed method specificity, sensitivity and linearity within a 2–10 µL/mL range. The Limit of Detection (LOD) and Limit of Quantification (LOQ) were found to be 0.0047 µL/mL and 0.0136 µL/mL, respectively. The residual solvent DMSO in the 1 mg of paliperidone nanocrystal sample was found to be 21.91 ppm. Greenness and whiteness evaluation were performed for the developed method.</div></div><div><h3>Conclusion</h3><div>This novel GC-FID method offers a robust and dependable analytical approach for the determination of residual solvents in paliperidone nanocrystals and has an application in the routine quality control analysis. Moreover, the method aligns with green analytical chemistry principles by incorporating low solvent consumption, reduced waste generation, and energy-efficient operation, thereby supporting environmentally sustainable pharmaceutical quality control.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"12 ","pages":"Article 100520"},"PeriodicalIF":4.1,"publicationDate":"2025-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144704834","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-07-18DOI: 10.1016/j.talo.2025.100522
Mohammed T. Shehabeldeen , Fotouh R. Mansour , Samah F. El-Malla , Aya A. Abdella
Automated in-tip dispersive micro-solid phase extraction is a miniaturized technique that could afford advantages of solid phase extraction with fewer steps and reduced environmental hazard. In this work, molecularly imprinted polymer was evaluated as a packing sorbent for a lab-made automated dispersive pipette tip extraction (MIP-DPX). The MIP was prepared using chitosan as the functional monomer, glutaraldehyde as the crosslinker, and ketoprofen (KTP) as the template molecule. The efficiency of KTP extraction using the devised automated tip was studied by investigating the effect of adsorption pH, elution volume, and the number of aspirating/dispensing cycles. High recovery rates were obtained at pH 4 employing 8 cycles of aspiration followed by KTP elution using methanol (500 μL) in a single dispensing cycle. The developed MIP-DPX demonstrated good linearity and reproducibility, making it suitable for KTP determination in environmental water. MIP-DPX was evaluated for environmental friendliness using the Complex Green Analytical Procedure Index (Complex GAPI) and Analytical GREEnness metric (AGREE), as well as practicality using the Blue Applicability Grade Index (BAGI). The developed workflow was proved to be a practical, environmentally friendly, and economic approach for pre-concentration and determination of KTP. The devised in-tip extraction system showed promising results paving the way for expanding the applicability of MIP-based SPE towards their automation.
{"title":"Automated MIP-based in-tip dispersive micro-solid phase extraction for determination of ketoprofen in environmental water: A proof of concept and performance evaluation","authors":"Mohammed T. Shehabeldeen , Fotouh R. Mansour , Samah F. El-Malla , Aya A. Abdella","doi":"10.1016/j.talo.2025.100522","DOIUrl":"10.1016/j.talo.2025.100522","url":null,"abstract":"<div><div>Automated in-tip dispersive micro-solid phase extraction is a miniaturized technique that could afford advantages of solid phase extraction with fewer steps and reduced environmental hazard. In this work, molecularly imprinted polymer was evaluated as a packing sorbent for a lab-made automated dispersive pipette tip extraction (MIP-DPX). The MIP was prepared using chitosan as the functional monomer, glutaraldehyde as the crosslinker, and ketoprofen (KTP) as the template molecule. The efficiency of KTP extraction using the devised automated tip was studied by investigating the effect of adsorption pH, elution volume, and the number of aspirating/dispensing cycles. High recovery rates were obtained at pH 4 employing 8 cycles of aspiration followed by KTP elution using methanol (500 μL) in a single dispensing cycle. The developed MIP-DPX demonstrated good linearity and reproducibility, making it suitable for KTP determination in environmental water. MIP-DPX was evaluated for environmental friendliness using the Complex Green Analytical Procedure Index (Complex GAPI) and Analytical GREEnness metric (AGREE), as well as practicality using the Blue Applicability Grade Index (BAGI). The developed workflow was proved to be a practical, environmentally friendly, and economic approach for pre-concentration and determination of KTP. The devised in-tip extraction system showed promising results paving the way for expanding the applicability of MIP-based SPE towards their automation.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"12 ","pages":"Article 100522"},"PeriodicalIF":4.1,"publicationDate":"2025-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144702811","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-07-18DOI: 10.1016/j.talo.2025.100521
Yang Xu , Ke Cao , Tao Huang , Yan Zhang , Cuixia Guo , Yuxuan Yang , Yonghong He , Xiaojun Luo , Defa Li
Pertussis, a highly contagious respiratory disease caused by Bordetella pertussis, remains a significant global health challenge despite vaccination efforts. China has witnessed a resurgence of cases, especially among young children. The diverse clinical manifestations and non-specific symptoms hinder early diagnosis. This study utilized quantitative proteomics analysis to explore differential protein expression in pertussis bacteremia, pneumonia, and non-complicated cases. The key findings include distinct protein profiles across different infection types, which suggest potential biomarkers and offer insights into disease severity and progression. Specifically, proteins such as ADH6 and TTC38 were significantly upregulated in pertussis sepsis, while LRRC42 was downregulated in pertussis pneumonia. During the progression of pertussis sepsis, NCOA3 increased and KCRS decreased from disease onset to improvement, and SAA2 surged in the recovery stage. In comparing pertussis sepsis patients with different outcomes, PTMS, NNMT, and ASSY were downregulated in the deceased patient.These findings enhance our understanding of pertussis pathogenesis, providing crucial insights for the development of more effective vaccines, diagnostics, and treatments, ultimately aiming to reduce the global burden of this infectious disease.
{"title":"Quantitative proteomics analysis of pertussis: Uncovering biomarkers for diagnosis and disease monitoring and insights into pathogenesis","authors":"Yang Xu , Ke Cao , Tao Huang , Yan Zhang , Cuixia Guo , Yuxuan Yang , Yonghong He , Xiaojun Luo , Defa Li","doi":"10.1016/j.talo.2025.100521","DOIUrl":"10.1016/j.talo.2025.100521","url":null,"abstract":"<div><div>Pertussis, a highly contagious respiratory disease caused by Bordetella pertussis, remains a significant global health challenge despite vaccination efforts. China has witnessed a resurgence of cases, especially among young children. The diverse clinical manifestations and non-specific symptoms hinder early diagnosis. This study utilized quantitative proteomics analysis to explore differential protein expression in pertussis bacteremia, pneumonia, and non-complicated cases. The key findings include distinct protein profiles across different infection types, which suggest potential biomarkers and offer insights into disease severity and progression. Specifically, proteins such as ADH6 and TTC38 were significantly upregulated in pertussis sepsis, while LRRC42 was downregulated in pertussis pneumonia. During the progression of pertussis sepsis, NCOA3 increased and KCRS decreased from disease onset to improvement, and SAA2 surged in the recovery stage. In comparing pertussis sepsis patients with different outcomes, PTMS, NNMT, and ASSY were downregulated in the deceased patient.These findings enhance our understanding of pertussis pathogenesis, providing crucial insights for the development of more effective vaccines, diagnostics, and treatments, ultimately aiming to reduce the global burden of this infectious disease.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"12 ","pages":"Article 100521"},"PeriodicalIF":4.1,"publicationDate":"2025-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144687226","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-07-18DOI: 10.1016/j.talo.2025.100519
Ola G. Hussein , Amr M. Mahmoud , Aya A. Mouhamed , Yan Dou , Qiong Nian , Nardine Safwat
Nanozymes engineered to mimic natural enzyme catalysis have emerged as promising alternatives due to their enhanced stability, cost-effectiveness, and tunable catalytic properties compared to biological enzymes. Developing nanozymes with well-defined porous structures and heteroatom doping is key to improving catalytic efficiency and selectivity particularly for applications in biosensing. Nanotechnology has become a key enabler in advancing catalysis, biosensing, and environmental monitoring thanks to the exceptional properties of nanomaterials such as large surface area, customizable optical characteristics, and enhanced catalytic activity. In this study, a novel nanozyme platform based on creatinine–thiourea–FeCl3 nanoparticles (CTF-NPs) was developed via a one-step pyrolysis method using colloidal silica as a porosity template. The synthesized CTF-NPs were uniformly structured as confirmed by SEM, EDX, FT-IR, UV–Vis, and XRD and featured effective nitrogen, sulfur, and iron doping contributing to their catalytic efficiency. The CTF-NPs exhibited strong peroxidase-like activity catalyzing the colorimetric oxidation of o-phenylenediamine (OPD) in the presence of hydrogen peroxide (H2O2). Kinetic studies revealed a Km of 0.819 mM and a Vmax of 1.620 μM/min outperforming several previously reported nanozyme systems. The sensor displayed a linear detection range of 10–700 μM for H2O2 with an excellent correlation coefficient (r= 0.9975) optimal at pH 4, 40 °C, and 10-minute incubation. Upon coupling with glucose oxidase (GOx), the platform enabled indirect glucose detection via enzymatically generated H2O2 showing a linear range of 100–600 μM with a correlation coefficient of r= 0.9953. The system exhibited high selectivity against common interferents, reproducible fabrication, and reliable performance in spiked human serum samples. Integration of the nanozyme system with a portable RGB color sensor (TCS34725) enabled quantitative, user-friendly, and instrument-free detection supporting the development of accessible point-of-care diagnostics. This work introduces a scalable and robust platform for glucose monitoring with promising implications for diabetes management and decentralized healthcare.
{"title":"Arduino-based portable point-of-care colorimetric glucose biosensor using nanozyme with enhanced peroxidase-like activity","authors":"Ola G. Hussein , Amr M. Mahmoud , Aya A. Mouhamed , Yan Dou , Qiong Nian , Nardine Safwat","doi":"10.1016/j.talo.2025.100519","DOIUrl":"10.1016/j.talo.2025.100519","url":null,"abstract":"<div><div>Nanozymes engineered to mimic natural enzyme catalysis have emerged as promising alternatives due to their enhanced stability, cost-effectiveness, and tunable catalytic properties compared to biological enzymes. Developing nanozymes with well-defined porous structures and heteroatom doping is key to improving catalytic efficiency and selectivity particularly for applications in biosensing. Nanotechnology has become a key enabler in advancing catalysis, biosensing, and environmental monitoring thanks to the exceptional properties of nanomaterials such as large surface area, customizable optical characteristics, and enhanced catalytic activity. In this study, a novel nanozyme platform based on creatinine–thiourea–FeCl<sub>3</sub> nanoparticles (CTF-NPs) was developed via a one-step pyrolysis method using colloidal silica as a porosity template. The synthesized CTF-NPs were uniformly structured as confirmed by SEM, EDX, FT-IR, UV–Vis, and XRD and featured effective nitrogen, sulfur, and iron doping contributing to their catalytic efficiency. The CTF-NPs exhibited strong peroxidase-like activity catalyzing the colorimetric oxidation of <em>o</em>-phenylenediamine (OPD) in the presence of hydrogen peroxide (H<sub>2</sub>O<sub>2</sub>). Kinetic studies revealed a K<sub>m</sub> of 0.819 mM and a V<sub>max</sub> of 1.620 μM/min outperforming several previously reported nanozyme systems. The sensor displayed a linear detection range of 10–700 μM for H<sub>2</sub>O<sub>2</sub> with an excellent correlation coefficient (r= 0.9975) optimal at pH 4<strong>,</strong> 40 °C<strong>,</strong> and 10-minute incubation. Upon coupling with glucose oxidase (GOx), the platform enabled indirect glucose detection via enzymatically generated H<sub>2</sub>O<sub>2</sub> showing a linear range of 100–600 μM with a correlation coefficient of r= 0.9953. The system exhibited high selectivity against common interferents, reproducible fabrication, and reliable performance in spiked human serum samples. Integration of the nanozyme system with a portable RGB color sensor (TCS34725) enabled quantitative, user-friendly, and instrument-free detection supporting the development of accessible point-of-care diagnostics. This work introduces a scalable and robust platform for glucose monitoring with promising implications for diabetes management and decentralized healthcare.</div></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":"12 ","pages":"Article 100519"},"PeriodicalIF":4.1,"publicationDate":"2025-07-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144702810","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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