Pub Date : 2026-01-30DOI: 10.1016/j.aca.2026.345139
Xueting Cui , Jun Wang , Tingyu Hou , Ming Cai , Luozhao Wang , Yanna Liu , Jinhua Li
Eutrophication of surface freshwater drinking sources intensifies, leading blue-green algae to release massive microcystins. Microcystin-LR (MC-LR), the most toxic variant, poses severe threats to public health and environmental safety. Conventional MC-LR detection methods rely on bulky, expensive equipment and involve complex, time-consuming sample pretreatment, making them unsuitable for on-site testing. This study developed a colorimetric sensing platform based on the binding of positively charged gold nanoparticles (AuNPs) to MC-LR aptamers for simple and rapid MC-LR detection. Without MC-LR, positively charged gold nanoparticles bind to negatively charged aptamers, aggregate, and turn the solution from yellow to white. This method exhibits high sensitivity (detection limit: 0.1 μg/L) and good specificity (insensitive to interferents like MC-YR and MC-RR), with a total assay time of 55 min, providing a rapid alternative to conventional laboratory-based methods like ELISA. Tests on actual water samples showed recoveries of 96.1–119.8% with relative standard deviations <10%, demonstrating good accuracy and precision for real environmental water analysis. The method's performance suggests its potential for on-site screening, although some variability was observed in complex matrices. This visualized assay eliminates reliance on large instruments, shortens detection time, and holds great potential for environmental water sample testing.
{"title":"Establishment of a rapid colorimetric sensor for Microcystin-LR based on specific aptamer and positively charged gold nanoparticles","authors":"Xueting Cui , Jun Wang , Tingyu Hou , Ming Cai , Luozhao Wang , Yanna Liu , Jinhua Li","doi":"10.1016/j.aca.2026.345139","DOIUrl":"10.1016/j.aca.2026.345139","url":null,"abstract":"<div><div>Eutrophication of surface freshwater drinking sources intensifies, leading blue-green algae to release massive microcystins. Microcystin-LR (MC-LR), the most toxic variant, poses severe threats to public health and environmental safety. Conventional MC-LR detection methods rely on bulky, expensive equipment and involve complex, time-consuming sample pretreatment, making them unsuitable for on-site testing. This study developed a colorimetric sensing platform based on the binding of positively charged gold nanoparticles (AuNPs) to MC-LR aptamers for simple and rapid MC-LR detection. Without MC-LR, positively charged gold nanoparticles bind to negatively charged aptamers, aggregate, and turn the solution from yellow to white. This method exhibits high sensitivity (detection limit: 0.1 μg/L) and good specificity (insensitive to interferents like MC-YR and MC-RR), with a total assay time of 55 min, providing a rapid alternative to conventional laboratory-based methods like ELISA. Tests on actual water samples showed recoveries of 96.1–119.8% with relative standard deviations <10%, demonstrating good accuracy and precision for real environmental water analysis. The method's performance suggests its potential for on-site screening, although some variability was observed in complex matrices. This visualized assay eliminates reliance on large instruments, shortens detection time, and holds great potential for environmental water sample testing.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1392 ","pages":"Article 345139"},"PeriodicalIF":6.0,"publicationDate":"2026-01-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146072867","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}
Pub Date : 2026-01-29DOI: 10.1016/j.aca.2026.345144
Ruxuan Mo, Chao Kang, Jianping Yuan, Carl Redshaw, Ying Huang, Qilong Zhang, Xiufang Yan
{"title":"A Near-Infrared Ratiometric Fluorescent Probe for Visual Sensing of H2S and Monitoring Its Fluctuation in Plant Roots under Drought and Flooding Stresses","authors":"Ruxuan Mo, Chao Kang, Jianping Yuan, Carl Redshaw, Ying Huang, Qilong Zhang, Xiufang Yan","doi":"10.1016/j.aca.2026.345144","DOIUrl":"https://doi.org/10.1016/j.aca.2026.345144","url":null,"abstract":"","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"117 1","pages":""},"PeriodicalIF":6.2,"publicationDate":"2026-01-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146072873","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}
Pub Date : 2026-01-29DOI: 10.1016/j.aca.2026.345140
Iuliia A. Poimenova, Elizaveta Yu. Zhukova, Svetlana T. Ovseenko, Nikita S. Saratovsky, Ivan K. Kiryukhin, Daria-Mariia V. Ratova, Dmitrii M. Filatov, Anastasia M. Alekseeva, Svetlana V. Smirnova, Mikhail A. Proskurnin, Ivan V. Mikheev
{"title":"Detailed impurity profiling of graphene oxide fractions by robust inductively coupled plasma optical emission spectrometry monitoring","authors":"Iuliia A. Poimenova, Elizaveta Yu. Zhukova, Svetlana T. Ovseenko, Nikita S. Saratovsky, Ivan K. Kiryukhin, Daria-Mariia V. Ratova, Dmitrii M. Filatov, Anastasia M. Alekseeva, Svetlana V. Smirnova, Mikhail A. Proskurnin, Ivan V. Mikheev","doi":"10.1016/j.aca.2026.345140","DOIUrl":"https://doi.org/10.1016/j.aca.2026.345140","url":null,"abstract":"","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"180 1","pages":"345140"},"PeriodicalIF":6.2,"publicationDate":"2026-01-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146072876","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}
Pub Date : 2026-01-29DOI: 10.1016/j.aca.2026.345162
L. Sanjuan-Navarro, P. Sanchis-Angulo, Y. Moliner-Martínez, P. Campíns-Falcó
Background
Silica materials vary widely in size, structure, and applicability, making their accurate characterization essential for ensuring proper performance across research and industrial applications. A strategy for hydrodynamic size assessment of silica materials ranging nanometers to micrometers is proposed here. Silica nanoparticles (SiO2NPs) of different sizes, halloysite as silica nanotubes, and silica obtained from rice straw combustion residues have been characterized employing asymmetrical flow field flow fractionation technique in combination with a DLS detector (AF4-DLS). Additional analyses were performed using scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR), and batch-mode DLS.
Results
Firstly, the different silica materials were dispersed using alkaline treatment. For halloysite, a detailed dispersibility assay was performed using a wide variety of compounds to identify optimal conditions for stable suspensions. The sizes of SiO2NPs obtained by AF4-DLS ranged between 15 and 200 nm, according to the type of NPs and their aggregation state. Halloysite exhibited sizes around 240–280 nm, corresponding to the transversal length. Additionally, the functionalization of this material with pigments was evaluated. As an example of micro material, silica extracted from combustion residues of rice straw was studied, resulting in average hydrodynamic diameters reaching up to 4 μm. Finally, analytical parameters were evaluated, and the results demonstrated suitable precision values, with limit of detection (LOD) in the range of 1.5∙10−4 % (w/v) to 7.2∙10−4 % (w/v).
Significance
These findings demonstrate the utility of the proposed AF4-DLS analytical strategy as an effective tool for silica characterization. By enabling assessment of hydrodynamic size across nanometer to micrometer scales, this approach enhances the understanding of particle behavior, aggregation, and functionalization, thereby supporting more informed decisions in the design and applications of silica materials.
{"title":"Size assessing of different silica-based materials by asymmetrical flow field flow fractionation: from nanometers to micrometers","authors":"L. Sanjuan-Navarro, P. Sanchis-Angulo, Y. Moliner-Martínez, P. Campíns-Falcó","doi":"10.1016/j.aca.2026.345162","DOIUrl":"10.1016/j.aca.2026.345162","url":null,"abstract":"<div><h3>Background</h3><div>Silica materials vary widely in size, structure, and applicability, making their accurate characterization essential for ensuring proper performance across research and industrial applications. A strategy for hydrodynamic size assessment of silica materials ranging nanometers to micrometers is proposed here. Silica nanoparticles (SiO<sub>2</sub>NPs) of different sizes, halloysite as silica nanotubes, and silica obtained from rice straw combustion residues have been characterized employing asymmetrical flow field flow fractionation technique in combination with a DLS detector (AF4-DLS). Additional analyses were performed using scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR), and batch-mode DLS.</div></div><div><h3>Results</h3><div>Firstly, the different silica materials were dispersed using alkaline treatment. For halloysite, a detailed dispersibility assay was performed using a wide variety of compounds to identify optimal conditions for stable suspensions. The sizes of SiO<sub>2</sub>NPs obtained by AF4-DLS ranged between 15 and 200 nm, according to the type of NPs and their aggregation state. Halloysite exhibited sizes around 240–280 nm, corresponding to the transversal length. Additionally, the functionalization of this material with pigments was evaluated. As an example of micro material, silica extracted from combustion residues of rice straw was studied, resulting in average hydrodynamic diameters reaching up to 4 μm. Finally, analytical parameters were evaluated, and the results demonstrated suitable precision values, with limit of detection (LOD) in the range of 1.5∙10<sup>−4</sup> % (w/v) to 7.2∙10<sup>−4</sup> % (w/v).</div></div><div><h3>Significance</h3><div>These findings demonstrate the utility of the proposed AF4-DLS analytical strategy as an effective tool for silica characterization. By enabling assessment of hydrodynamic size across nanometer to micrometer scales, this approach enhances the understanding of particle behavior, aggregation, and functionalization, thereby supporting more informed decisions in the design and applications of silica materials.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1391 ","pages":"Article 345162"},"PeriodicalIF":6.0,"publicationDate":"2026-01-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146072875","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}
Pub Date : 2026-01-27DOI: 10.1016/j.aca.2026.345159
Jorgelina Zaldarriaga-Heredia , Antonella E. Montemerlo , José M. Camiña , Mirta R. Alcaraz , Silvana M. Azcarate , Héctor C. Goicoechea
Background
The exploitation of multidimensional information represents a key challenge in analytical chemistry, particularly for classification tasks involving complex systems. This study systematically investigates the influence of data structure—ranging from first-to third-order—on classification performance using simulated and experimental fluorescence datasets. Chemometric models based on partial least squares–discriminant analysis (PLS-DA), multi-way PLS-DA (N-PLS-DA), and parallel factor analysis combined with discriminant analysis (PARAFAC-DA) were evaluated under varying conditions of class balance, noise, and sample size. Simulated and experimental datasets based on excitation–emission fluorescence spectroscopy were used.
Results
Simulated results demonstrated that increasing data dimensionality markedly enhanced discrimination ability, yielding higher accuracy and reduced error rates. Third-order models achieved average accuracies above 93 %, improving by up to 20 % and 10 % compared to the first- and second-order models, respectively. The methodology was further validated using excitation–emission fluorescence data from extra virgin and virgin olive oils subjected to infrared heating. Both N-PLS-DA and PARAFAC-DA provided successful discrimination, with PARAFAC-DA offering superior interpretability through chemically meaningful component profiles describing degradation and oxidation processes. Overall, the findings confirm that third-order chemometric models effectively integrate structural, spectral, and kinetic information, thereby improving classification reliability and interpretability. Even under conditions of class imbalance and limited sample availability, third-order models maintained low error rates and consistently high accuracy values, confirming their robustness and generalizability.
Significance
This study provides a comprehensive evaluation of how data structure influences multivariate classification performance. The proposed approach highlights the analytical potential of higher-order data modelling as a powerful and versatile strategy for classifying complex matrices. The findings firmly establish third-order modelling as a versatile and compelling tool for analytical applications where data complexity and real-world variability are unavoidable.
{"title":"Multi-way data modelling for enhancing classification performance: Fluorescence data as a case of study","authors":"Jorgelina Zaldarriaga-Heredia , Antonella E. Montemerlo , José M. Camiña , Mirta R. Alcaraz , Silvana M. Azcarate , Héctor C. Goicoechea","doi":"10.1016/j.aca.2026.345159","DOIUrl":"10.1016/j.aca.2026.345159","url":null,"abstract":"<div><h3>Background</h3><div>The exploitation of multidimensional information represents a key challenge in analytical chemistry, particularly for classification tasks involving complex systems. This study systematically investigates the influence of data structure—ranging from first-to third-order—on classification performance using simulated and experimental fluorescence datasets. Chemometric models based on partial least squares–discriminant analysis (PLS-DA), multi-way PLS-DA (N-PLS-DA), and parallel factor analysis combined with discriminant analysis (PARAFAC-DA) were evaluated under varying conditions of class balance, noise, and sample size. Simulated and experimental datasets based on excitation–emission fluorescence spectroscopy were used.</div></div><div><h3>Results</h3><div>Simulated results demonstrated that increasing data dimensionality markedly enhanced discrimination ability, yielding higher accuracy and reduced error rates. Third-order models achieved average accuracies above 93 %, improving by up to 20 % and 10 % compared to the first- and second-order models, respectively. The methodology was further validated using excitation–emission fluorescence data from extra virgin and virgin olive oils subjected to infrared heating. Both N-PLS-DA and PARAFAC-DA provided successful discrimination, with PARAFAC-DA offering superior interpretability through chemically meaningful component profiles describing degradation and oxidation processes. Overall, the findings confirm that third-order chemometric models effectively integrate structural, spectral, and kinetic information, thereby improving classification reliability and interpretability. Even under conditions of class imbalance and limited sample availability, third-order models maintained low error rates and consistently high accuracy values, confirming their robustness and generalizability.</div></div><div><h3>Significance</h3><div>This study provides a comprehensive evaluation of how data structure influences multivariate classification performance. The proposed approach highlights the analytical potential of higher-order data modelling as a powerful and versatile strategy for classifying complex matrices. The findings firmly establish third-order modelling as a versatile and compelling tool for analytical applications where data complexity and real-world variability are unavoidable.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1391 ","pages":"Article 345159"},"PeriodicalIF":6.0,"publicationDate":"2026-01-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146056528","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}
Pub Date : 2026-01-26DOI: 10.1016/j.aca.2026.345158
Yongfang Li , Xuan Chen , Zhexun Yang , Zijun Wang , Rui Wang
Rapid and ultrasensitive detection of Vibrio parahaemolyticus (V. parahaemolyticus, Vp) is of great significance for the early prevention of foodborne disease. Traditional methods for detecting Vp are time-consuming, exhibiting low sensitivity and specificity. In this study, CRISPR/Cas12a system is integrated with electrochemical sensing and polymerase chain reaction (PCR) to establish a PCR-based E-CRISPR biosensor for Vp detection. The target DNA extracted from Vp is amplified by PCR, then activate CRISPR/Cas12a system to cleave methylene blue (MB)-labeled hairpin DNA probes on electrode, resulting in great changes in current. The employment of hairpin DNA probes reduces the steric hindrance for Cas12a trans-cleavage, acquiring a better cleavage efficiency and sensing performance. Under optimal conditions, the limit of detection reaches 1.17 copies/μL (genomic DNA), 1.23 CFU/mL (standard bacteria), and 12.3 CFU/g (artificially contaminated shrimp samples) respectively. Moreover, the PCR-based E-CRISPR biosensor demonstrates superior reproducibility and specificity. Most importantly, the E-CRISPR biosensor were in 100 % agreement with real time quantitative PCR for the detection of 18 seafood samples, which confirms the biosensor's broad applicability for monitoring Vp in complex food matrix. Our developed E-CRISPR biosensor demonstrates to be a simple, rapid and ultrasensitive method for Vp detection in the food supply chain, and can be extended to other foodborne pathogens.
{"title":"CRISPR/Cas12a empowered electrochemical biosensor for ultrasensitive detection of Vibrio parahaemolyticus in seafood samples","authors":"Yongfang Li , Xuan Chen , Zhexun Yang , Zijun Wang , Rui Wang","doi":"10.1016/j.aca.2026.345158","DOIUrl":"10.1016/j.aca.2026.345158","url":null,"abstract":"<div><div>Rapid and ultrasensitive detection of <em>Vibrio parahaemolyticus</em> (<em>V. parahaemolyticus</em>, V<em>p</em>) is of great significance for the early prevention of foodborne disease. Traditional methods for detecting V<em>p</em> are time-consuming, exhibiting low sensitivity and specificity. In this study, CRISPR/Cas12a system is integrated with electrochemical sensing and polymerase chain reaction (PCR) to establish a PCR-based E-CRISPR biosensor for V<em>p</em> detection. The target DNA extracted from V<em>p</em> is amplified by PCR, then activate CRISPR/Cas12a system to cleave methylene blue (MB)-labeled hairpin DNA probes on electrode, resulting in great changes in current. The employment of hairpin DNA probes reduces the steric hindrance for Cas12a <em>trans</em>-cleavage, acquiring a better cleavage efficiency and sensing performance. Under optimal conditions, the limit of detection reaches 1.17 copies/μL (genomic DNA), 1.23 CFU/mL (standard bacteria), and 12.3 CFU/g (artificially contaminated shrimp samples) respectively. Moreover, the PCR-based E-CRISPR biosensor demonstrates superior reproducibility and specificity. Most importantly, the E-CRISPR biosensor were in 100 % agreement with real time quantitative PCR for the detection of 18 seafood samples, which confirms the biosensor's broad applicability for monitoring V<em>p</em> in complex food matrix. Our developed E-CRISPR biosensor demonstrates to be a simple, rapid and ultrasensitive method for V<em>p</em> detection in the food supply chain, and can be extended to other foodborne pathogens.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1391 ","pages":"Article 345158"},"PeriodicalIF":6.0,"publicationDate":"2026-01-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146048632","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}
Glutathione (GSH), the most abundant cellular non-protein thiol and a central antioxidant, plays essential roles in regulating redox homeostasis, signal transduction, and detoxification processes. Altered GSH levels are closely associated with various pathological conditions, including neurodegenerative disorders, and liver injury. Notably, tumor tissues exhibit markedly elevated GSH concentrations (up to 4–10 times higher than in normal cells), where it promotes tumor proliferation, invasion, and chemoresistance by sustaining a reduced microenvironment, these characteristics make GSH an important biomarker and therapeutic target in oncology.
Results
We developed a novel “switch-on” near-infrared (NIR) fluorescence nanoprobe, Ag2S–CH@Cu-TCPP, for the highly sensitive and selective detection and imaging of GSH. The nanoprobe was constructed by conjugating histidine-rich CH peptides to carboxyl-capped Ag2S quantum dots (Ag2S QDs), which were then self-assembled onto two-dimensional Cu-TCPP metal-organic framework (MOF) nanosheets via coordination between Cu2+ and imidazole groups. In this design, Cu-TCPP acts as an efficient quencher for the Ag2S–CH fluorescence via a fluorescence resonance energy transfer (FRET) mechanism. Upon encountering GSH, the reduction of Cu2+ to Cu + disrupts the FRET process, leading to the recovery of the NIR fluorescence signal. This nanoprobe demonstrated a low detection limit of 5.33 μM and a wide linear range from 0.625 to 10 mM for GSH quantification, with excellent selectivity, high reproducibility, and favorable biocompatibility. We successfully applied the platform for monitoring intracellular GSH levels and distinguishing between cancer cells and normal cells based on their differential GSH expression.
Significance and novelty
The “switch-on” probe demonstrates excellent biocompatibility and is applicable for cellular imaging. It enables discrimination between normal and cancer cells while supporting semi-quantitative analysis of both endogenous and exogenous GSH. This work provides a novel and reliable strategy for tumor diagnosis and advanced investigations into GSH-related biological processes.
{"title":"A peptide-functionalized quantum Dots/MOF nanosheets fluorescence biosensor for glutathione sensing and cellular imaging","authors":"Tongfang Chen , Jingjie Liang , Weiqing Liu , Fengxia Zhou , Chanci Qiu , Yuhui Peng , Xie Zhou","doi":"10.1016/j.aca.2026.345120","DOIUrl":"10.1016/j.aca.2026.345120","url":null,"abstract":"<div><h3>Background</h3><div>Glutathione (GSH), the most abundant cellular non-protein thiol and a central antioxidant, plays essential roles in regulating redox homeostasis, signal transduction, and detoxification processes. Altered GSH levels are closely associated with various pathological conditions, including neurodegenerative disorders, and liver injury. Notably, tumor tissues exhibit markedly elevated GSH concentrations (up to 4–10 times higher than in normal cells), where it promotes tumor proliferation, invasion, and chemoresistance by sustaining a reduced microenvironment, these characteristics make GSH an important biomarker and therapeutic target in oncology.</div></div><div><h3>Results</h3><div>We developed a novel “switch-on” near-infrared (NIR) fluorescence nanoprobe, Ag<sub>2</sub>S–CH@Cu-TCPP, for the highly sensitive and selective detection and imaging of GSH. The nanoprobe was constructed by conjugating histidine-rich CH peptides to carboxyl-capped Ag<sub>2</sub>S quantum dots (Ag<sub>2</sub>S QDs), which were then self-assembled onto two-dimensional Cu-TCPP metal-organic framework (MOF) nanosheets via coordination between Cu<sup>2+</sup> and imidazole groups. In this design, Cu-TCPP acts as an efficient quencher for the Ag<sub>2</sub>S–CH fluorescence via a fluorescence resonance energy transfer (FRET) mechanism. Upon encountering GSH, the reduction of Cu<sup>2+</sup> to Cu <sup>+</sup> disrupts the FRET process, leading to the recovery of the NIR fluorescence signal. This nanoprobe demonstrated a low detection limit of 5.33 μM and a wide linear range from 0.625 to 10 mM for GSH quantification, with excellent selectivity, high reproducibility, and favorable biocompatibility. We successfully applied the platform for monitoring intracellular GSH levels and distinguishing between cancer cells and normal cells based on their differential GSH expression.</div></div><div><h3>Significance and novelty</h3><div>The “switch-on” probe demonstrates excellent biocompatibility and is applicable for cellular imaging. It enables discrimination between normal and cancer cells while supporting semi-quantitative analysis of both endogenous and exogenous GSH. This work provides a novel and reliable strategy for tumor diagnosis and advanced investigations into GSH-related biological processes.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1391 ","pages":"Article 345120"},"PeriodicalIF":6.0,"publicationDate":"2026-01-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146042957","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}
Pub Date : 2026-01-24DOI: 10.1016/j.aca.2026.345156
Karolina Ostrowska , Maria Mazurkiewicz-Bełdzińska , Jakub Szymarek , Sylwia Studzińska
Background
Antisense oligonucleotides are synthetic nucleic acid molecules capable of selectively modulating gene expression. As the number of approved antisense oligonucleotide therapies grows, reliable analytical procedures are needed to monitor their pharmacokinetics, metabolism, and safety. Current solid phase extraction strategies often suffer from limited recovery or poor reproducibility. Methods using non-polar, hydrophilic or anion-exchange sorbents, require application of ion-pair reagents, or high concentration of salts or long conditioning. On the other hand, the potential of sorbents with hydrophobic-hydrophilic properties used for mixed-mode extraction remains unexplored. Our study presents the first application of newly synthesized materials for the isolation of therapeutic antisense oligonucleotides from cerebrospinal fluid samples.
Results
Five silica-based sorbents modified with aminopropyl, aliphatic, aromatic, and dicarboxylic groups were designed, synthesized, and characterized. The functionalization of sorbents enables various interactions with oligonucleotides, namely electrostatic, hydrophobic, π … π interactions, and hydrogen bonding. A new, mixed-mode dispersive solid phase extraction procedure was developed using a central composite design, enabling a systematic evaluation of the factors governing antisense oligonucleotide desorption. The effectiveness of the procedure was assessed for oligonucleotides varying in chemical modification and length. Recoveries depended on both factors and were the highest for shortmers with 2′-O-methyl modification. This effect is advantageous for the extraction of antisense oligonucleotide metabolites. The developed method was successfully used for the extraction of antisense oligonucleotides from cerebrospinal fluid, enabling reproducible recoveries (40–93 %). The matrix effects ranged from 89 % to 100 %. The highest recoveries were obtained for an oligonucleotide modified at two structural elements, making the method advantageous for the extraction of oligonucleotides used in therapy.
Significance
The proposed mixed-mode dispersive solid-phase extraction procedure provides a simple, fast, and reproducible approach for isolating of antisense oligonucleotides from cerebrospinal fluid. The method significantly simplifies sample preparation, since the procedure may be straightforwardly applied without additional purification steps. These results for the first time demonstrate the suitability and high analytical potential of hydrophobic-hydrophilic sorbents for the extraction of antisense oligonucleotides from biological samples.
反义寡核苷酸是一种能够选择性调节基因表达的合成核酸分子。随着批准的反义寡核苷酸疗法数量的增加，需要可靠的分析方法来监测它们的药代动力学、代谢和安全性。目前的固相萃取策略往往存在回收率有限或重现性差的问题。使用非极性、亲水性或阴离子交换吸附剂的方法，需要使用离子对试剂，或高浓度的盐或长时间的调理。另一方面，具有疏亲水性的吸附剂用于混合模式萃取的潜力仍未得到探索。我们的研究首次应用新合成的材料从脑脊液样品中分离治疗性反义寡核苷酸。结果设计、合成了氨基丙基、脂肪基、芳香族和二羧基改性的5种硅基吸附剂，并对其进行了表征。吸附剂的功能化可以实现与寡核苷酸的各种相互作用，即静电、疏水、π…π相互作用和氢键。采用中心复合设计，开发了一种新的混合模式分散固相萃取方法，能够系统地评估控制反义寡核苷酸解吸的因素。对不同化学修饰和长度的寡核苷酸的有效性进行了评估。回收率取决于这两个因素，并且对2 ' - o -甲基改性的短链剂的回收率最高。这一效应有利于反义寡核苷酸代谢物的提取。该方法成功地用于从脑脊液中提取反义寡核苷酸，具有可重复性（40 - 93%）。基质效应从89%到100%不等。在两个结构元素修饰的寡核苷酸中获得了最高的回收率，使该方法有利于提取用于治疗的寡核苷酸。意义所提出的混合模式色散固相萃取方法为脑脊液中反义寡核苷酸的分离提供了一种简单、快速、可重复性好的方法。该方法大大简化了样品制备，因为该程序可以直接应用，而无需额外的纯化步骤。这些结果首次证明了疏水-亲水吸附剂在生物样品中反义寡核苷酸提取中的适用性和较高的分析潜力。
{"title":"Synthesis, characterization, and application of sorbents for the mixed-mode extraction of antisense oligonucleotides from cerebrospinal fluid samples","authors":"Karolina Ostrowska , Maria Mazurkiewicz-Bełdzińska , Jakub Szymarek , Sylwia Studzińska","doi":"10.1016/j.aca.2026.345156","DOIUrl":"10.1016/j.aca.2026.345156","url":null,"abstract":"<div><h3>Background</h3><div>Antisense oligonucleotides are synthetic nucleic acid molecules capable of selectively modulating gene expression. As the number of approved antisense oligonucleotide therapies grows, reliable analytical procedures are needed to monitor their pharmacokinetics, metabolism, and safety. Current solid phase extraction strategies often suffer from limited recovery or poor reproducibility. Methods using non-polar, hydrophilic or anion-exchange sorbents, require application of ion-pair reagents, or high concentration of salts or long conditioning. On the other hand, the potential of sorbents with hydrophobic-hydrophilic properties used for mixed-mode extraction remains unexplored. Our study presents the first application of newly synthesized materials for the isolation of therapeutic antisense oligonucleotides from cerebrospinal fluid samples.</div></div><div><h3>Results</h3><div>Five silica-based sorbents modified with aminopropyl, aliphatic, aromatic, and dicarboxylic groups were designed, synthesized, and characterized. The functionalization of sorbents enables various interactions with oligonucleotides, namely electrostatic, hydrophobic, π … π interactions, and hydrogen bonding. A new, mixed-mode dispersive solid phase extraction procedure was developed using a central composite design, enabling a systematic evaluation of the factors governing antisense oligonucleotide desorption. The effectiveness of the procedure was assessed for oligonucleotides varying in chemical modification and length. Recoveries depended on both factors and were the highest for shortmers with 2′-O-methyl modification. This effect is advantageous for the extraction of antisense oligonucleotide metabolites. The developed method was successfully used for the extraction of antisense oligonucleotides from cerebrospinal fluid, enabling reproducible recoveries (40–93 %). The matrix effects ranged from 89 % to 100 %. The highest recoveries were obtained for an oligonucleotide modified at two structural elements, making the method advantageous for the extraction of oligonucleotides used in therapy.</div></div><div><h3>Significance</h3><div>The proposed mixed-mode dispersive solid-phase extraction procedure provides a simple, fast, and reproducible approach for isolating of antisense oligonucleotides from cerebrospinal fluid. The method significantly simplifies sample preparation, since the procedure may be straightforwardly applied without additional purification steps. These results for the first time demonstrate the suitability and high analytical potential of hydrophobic-hydrophilic sorbents for the extraction of antisense oligonucleotides from biological samples.</div></div>","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"1391 ","pages":"Article 345156"},"PeriodicalIF":6.0,"publicationDate":"2026-01-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146048634","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}
Pub Date : 2026-01-24DOI: 10.1016/j.aca.2026.345155
Alejandro C. Olivieri
{"title":"Old advice on multivariate calibration: still in force, but not always followed. A tutorial.","authors":"Alejandro C. Olivieri","doi":"10.1016/j.aca.2026.345155","DOIUrl":"https://doi.org/10.1016/j.aca.2026.345155","url":null,"abstract":"","PeriodicalId":240,"journal":{"name":"Analytica Chimica Acta","volume":"36 1","pages":""},"PeriodicalIF":6.2,"publicationDate":"2026-01-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146048633","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}
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