Pub Date : 2025-10-01Epub Date: 2025-08-20DOI: 10.1016/j.sampre.2025.100207
Vincenzo Mazzaracchio , Christian Gosti , Laura Belcastro , Fabiana Arduini
Since 2009, paper-based electrochemical biosensors have demonstrated several additional features in analytical chemistry thanks to their capability to manage the fluids by pump-free microfluidics, easily preconcentrate the target analytes, treat the sample with a task-free approach, and detect the target analyte with high sensitivity and accuracy. Herein, we point out the use of paper as a functional material for sample preparation, addressing easily and in a sustainable way the fluid sample management, filtration, separation, centrifugation, chemical sample treatment, and reagent addition. The use of paper for sample preparation in the electrochemical (bio)sensor field is shed light for the first time in a dedicated review. The overriding goal is to highlight the advantages of these cost-effective, environmentally friendly, and easy-to-use devices for smart preparation procedures and accurate electrochemical detection of the target analytes in several fields, including biomedical, environmental, and agrifood.
{"title":"Paper as an ecodesigned and smart material for sample preparation integrated with electrochemical (bio)sensors","authors":"Vincenzo Mazzaracchio , Christian Gosti , Laura Belcastro , Fabiana Arduini","doi":"10.1016/j.sampre.2025.100207","DOIUrl":"10.1016/j.sampre.2025.100207","url":null,"abstract":"<div><div>Since 2009, paper-based electrochemical biosensors have demonstrated several additional features in analytical chemistry thanks to their capability to manage the fluids by pump-free microfluidics, easily preconcentrate the target analytes, treat the sample with a task-free approach, and detect the target analyte with high sensitivity and accuracy. Herein, we point out the use of paper as a functional material for sample preparation, addressing easily and in a sustainable way the fluid sample management, filtration, separation, centrifugation, chemical sample treatment, and reagent addition. The use of paper for sample preparation in the electrochemical (bio)sensor field is shed light for the first time in a dedicated review. The overriding goal is to highlight the advantages of these cost-effective, environmentally friendly, and easy-to-use devices for smart preparation procedures and accurate electrochemical detection of the target analytes in several fields, including biomedical, environmental, and agrifood.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100207"},"PeriodicalIF":6.5,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144989996","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 : 2025-10-01Epub Date: 2025-11-20DOI: 10.1016/j.sampre.2025.100226
Ana M. Pedraza-Soto, Rafael Lucena, Soledad Cárdenas
Proteinaceous materials are useful precursors for preparing sustainable and cost-effective sorptive phases. Among them, chicken egg white is an excellent alternative, serving as a source of ovalbumin that can be used as a biosorbent. In this article, the combination of egg white with cellulose paper is evaluated to synthesize a planar protein-based sorptive phase with high porosity and surface area. For this purpose, the paper was dip-coated in egg-white, followed by thermal curing that induced protein denaturation and self-crosslinking. The preparation was quite simple and affordable, since it did not require subsequent functionalization procedures, allowing the preparation of 25 sorptive phases with only 1 mL of pasteurized egg white. The resulting egg-white paper (EW-paper) enabled the isolation of the analytes through a mixed-mode interaction mechanism, comprising both hydrophobic and cation-exchange interactions. This potential was corroborated by evaluating the extraction capacity of the EW-paper towards some selective serotonin reuptake inhibitors (SSRI) (fluoxetine, paroxetine, sertraline, and venlafaxine) from saliva samples. The analytes were finally determined by direct infusion mass spectrometry analysis. Once optimized, the method allows the determination of the target compounds in the low µgL-1 range, also fulfilling the validation criteria in terms of precision (better than 9.1 % and 11.8 % in intra- and inter-day precision, respectively) and accuracy (in the range 84 -118 %). Finally, the applicability of the method was demonstrated by analyzing real saliva samples from a patient under paroxetine treatment.
{"title":"Chicken egg white coated paper, a sustainable mixed-mode cationic exchange biocomposite to extract antidepressants from saliva samples prior to their determination by direct infusion mass spectrometry","authors":"Ana M. Pedraza-Soto, Rafael Lucena, Soledad Cárdenas","doi":"10.1016/j.sampre.2025.100226","DOIUrl":"10.1016/j.sampre.2025.100226","url":null,"abstract":"<div><div>Proteinaceous materials are useful precursors for preparing sustainable and cost-effective sorptive phases. Among them, chicken egg white is an excellent alternative, serving as a source of ovalbumin that can be used as a biosorbent. In this article, the combination of egg white with cellulose paper is evaluated to synthesize a planar protein-based sorptive phase with high porosity and surface area. For this purpose, the paper was dip-coated in egg-white, followed by thermal curing that induced protein denaturation and self-crosslinking. The preparation was quite simple and affordable, since it did not require subsequent functionalization procedures, allowing the preparation of 25 sorptive phases with only 1 mL of pasteurized egg white. The resulting egg-white paper (EW-paper) enabled the isolation of the analytes through a mixed-mode interaction mechanism, comprising both hydrophobic and cation-exchange interactions. This potential was corroborated by evaluating the extraction capacity of the EW-paper towards some selective serotonin reuptake inhibitors (SSRI) (fluoxetine, paroxetine, sertraline, and venlafaxine) from saliva samples. The analytes were finally determined by direct infusion mass spectrometry analysis. Once optimized, the method allows the determination of the target compounds in the low µgL<sup>-1</sup> range, also fulfilling the validation criteria in terms of precision (better than 9.1 % and 11.8 % in intra- and inter-day precision, respectively) and accuracy (in the range 84 -118 %). Finally, the applicability of the method was demonstrated by analyzing real saliva samples from a patient under paroxetine treatment.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100226"},"PeriodicalIF":6.5,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145623496","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 : 2025-10-01Epub Date: 2025-10-09DOI: 10.1016/j.sampre.2025.100216
Joaquim A. Nóbrega , Lorenzo Rossi , Gianpaolo Rota , Mirco Rossetti , Valentina Carrara , Camillo Pirola , Giulio Colnaghi , Diego Carnaroglio
Rapidly moving to the 3rd decade of the 21st century, it is clear that our technologies must evolve to sustainable processes, not aggressive to the environment nor to all forms of life. Chemical sciences are going green and surely analytical chemistry is moving towards this same direction. But we need to speed up the pace. To evaluate an analytical procedure, we should be able to validate it. Nowadays, method validation is not only the demonstration that analytical results are accurate, in fact method validation is also related to green chemistry aspects. If we think about elemental analysis, we can state that the sample preparation step has been improved, nonetheless it certainly requires further improvements through the development of greener procedures. In this contribution, we propose a set of green metrics named GreenPrep MW Score for the evaluation of microwave-assisted sample preparation procedures using different technologies, either based on cavity microwave oven, or on a single reaction chamber system. The GreenPrep MW Score was proposed considering the whole analytical procedure and how chemical parameters, technology variables and workflow can be optimized, and how these factors impact green metrics score. The authors do not intend to substitute sound metrics already proposed for evaluating the sample preparation step. Our goal is to propose a complementary strategy which helps us identify specific points to be improved in microwave-assisted procedures. The application of the developed metric was demonstrated for several samples containing different matrices, such as foods, multivitamin tablets, spodumene; in addition, strategies for improving green chemistry aspects were discussed.
{"title":"Green metric for microwave-assisted sample preparation for elemental analysis: GreenPrep MW Score","authors":"Joaquim A. Nóbrega , Lorenzo Rossi , Gianpaolo Rota , Mirco Rossetti , Valentina Carrara , Camillo Pirola , Giulio Colnaghi , Diego Carnaroglio","doi":"10.1016/j.sampre.2025.100216","DOIUrl":"10.1016/j.sampre.2025.100216","url":null,"abstract":"<div><div>Rapidly moving to the 3<sup>rd</sup> decade of the 21<sup>st</sup> century, it is clear that our technologies must evolve to sustainable processes, not aggressive to the environment nor to all forms of life. Chemical sciences are going green and surely analytical chemistry is moving towards this same direction. But we need to speed up the pace. To evaluate an analytical procedure, we should be able to validate it. Nowadays, method validation is not only the demonstration that analytical results are accurate, in fact method validation is also related to green chemistry aspects. If we think about elemental analysis, we can state that the sample preparation step has been improved, nonetheless it certainly requires further improvements through the development of greener procedures. In this contribution, we propose a set of green metrics named GreenPrep MW Score for the evaluation of microwave-assisted sample preparation procedures using different technologies, either based on cavity microwave oven, or on a single reaction chamber system. The GreenPrep MW Score was proposed considering the whole analytical procedure and how chemical parameters, technology variables and workflow can be optimized, and how these factors impact green metrics score. The authors do not intend to substitute sound metrics already proposed for evaluating the sample preparation step. Our goal is to propose a complementary strategy which helps us identify specific points to be improved in microwave-assisted procedures. The application of the developed metric was demonstrated for several samples containing different matrices, such as foods, multivitamin tablets, spodumene; in addition, strategies for improving green chemistry aspects were discussed.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100216"},"PeriodicalIF":6.5,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145333083","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 : 2025-10-01Epub Date: 2025-10-26DOI: 10.1016/j.sampre.2025.100220
Renan Vitek , Tahereh Tehrani , Laura Pont , María Vergara-Barberán , José Manuel Herrero-Martínez , Fernando Benavente , Jorge C. Masini
A novel polyhedral oligomeric silsesquioxane methacryl substituted (POSS-MA) monolithic microcartridge was prepared for the determination of low levels of the allergenic protein β-lactoglobulin (β-LG) in food by on-line solid-phase extraction capillary electrophoresis-mass spectrometry (SPE-CE-MS). The material was synthesized inside a 250 μm inner diameter (i.d.) capillary column by free radical polymerization using a simple "one-pot" method. This capillary column was subsequently cut and straightforwardly assembled as microcartridges connected in-line with 75 μm i.d. separation capillaries for SPE-CE-MS. Several SPE-CE-MS parameters (such as loading time, type of eluent, or time and pressure of elution) were optimized using an acidic background electrolyte (BGE) composed of 2 M acetic acid (HAc, pH 2.2). Under optimized conditions, the protein sample was loaded at 930 mbar for 20 min (ca. 110 μL), followed by a washing step with BGE at 930 mbar for 1 min, and finally eluted with 2 M HAc in methanol at 100 mbar for 60 s (ca. 600 nL). The method exhibited linearity from 0.25 to 10 μg·mL−1 of β-LG, with a limit of detection of 0.1 μg·mL−1, and a 100-fold increase in sensitivity compared to CE-MS. It was successfully applied to the determination of β-LG in dairy free white breads, yielding satisfactory results. These outcomes highlight the strong potential of the developed SPE-CE-MS method, using plug-and-play POSS-MA monolithic microcartridges, for precise food safety and quality control.
{"title":"Polyhedral oligomeric silsesquioxane hybrid monolithic microcartridges for the determination of β-lactoglobulin in food by on-line solid-phase extraction capillary electrophoresis-mass spectrometry","authors":"Renan Vitek , Tahereh Tehrani , Laura Pont , María Vergara-Barberán , José Manuel Herrero-Martínez , Fernando Benavente , Jorge C. Masini","doi":"10.1016/j.sampre.2025.100220","DOIUrl":"10.1016/j.sampre.2025.100220","url":null,"abstract":"<div><div>A novel polyhedral oligomeric silsesquioxane methacryl substituted (POSS-MA) monolithic microcartridge was prepared for the determination of low levels of the allergenic protein β-lactoglobulin (β-LG) in food by on-line solid-phase extraction capillary electrophoresis-mass spectrometry (SPE-CE-MS). The material was synthesized inside a 250 μm inner diameter (i.d.) capillary column by free radical polymerization using a simple \"one-pot\" method. This capillary column was subsequently cut and straightforwardly assembled as microcartridges connected in-line with 75 μm i.d. separation capillaries for SPE-CE-MS. Several SPE-CE-MS parameters (such as loading time, type of eluent, or time and pressure of elution) were optimized using an acidic background electrolyte (BGE) composed of 2 M acetic acid (HAc, pH 2.2). Under optimized conditions, the protein sample was loaded at 930 mbar for 20 min (<em>ca</em>. 110 μL), followed by a washing step with BGE at 930 mbar for 1 min, and finally eluted with 2 M HAc in methanol at 100 mbar for 60 s (<em>ca.</em> 600 nL). The method exhibited linearity from 0.25 to 10 μg·mL<sup>−1</sup> of β-LG, with a limit of detection of 0.1 μg·mL<sup>−1</sup>, and a 100-fold increase in sensitivity compared to CE-MS. It was successfully applied to the determination of β-LG in dairy free white breads, yielding satisfactory results. These outcomes highlight the strong potential of the developed SPE-CE-MS method, using plug-and-play POSS-MA monolithic microcartridges, for precise food safety and quality control.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100220"},"PeriodicalIF":6.5,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145473709","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 : 2025-08-01Epub Date: 2025-07-23DOI: 10.1016/j.sampre.2025.100202
P. García-Atienza, A. García-Juan, S. Armenta, J.M. Herrero-Martínez, H. Martínez-Pérez-Cejuela
The determination of drugs in biological fluids is essential across various fields, including toxicological analysis, pharmacokinetic studies, and the development of new pharmaceutical products, among others. However, the complexity of biological matrices—due to the presence of endogenous compounds and the typically low concentrations of target analytes—needs efficient sample preparation strategies alongside high-performance instrumentation to achieve the sensitivity and selectivity required in modern analytical chemistry. In response to these challenges, recent advancements have focused on the development of advanced solid materials and their integration with sample preparation techniques. This review highlights recent progress in sorbents with enhanced selectivity, engineered materials such as crystalline frameworks, and the use of biopolymers as natural sorbents for drug analysis in biofluids. Additionally, the application of 3D-printed materials for the fabrication of extraction devices is presented. The article also provides insights into emerging trends and future directions in this evolving field.
{"title":"Advanced solid materials for the extraction of drugs from biological fluids","authors":"P. García-Atienza, A. García-Juan, S. Armenta, J.M. Herrero-Martínez, H. Martínez-Pérez-Cejuela","doi":"10.1016/j.sampre.2025.100202","DOIUrl":"10.1016/j.sampre.2025.100202","url":null,"abstract":"<div><div>The determination of drugs in biological fluids is essential across various fields, including toxicological analysis, pharmacokinetic studies, and the development of new pharmaceutical products, among others. However, the complexity of biological matrices—due to the presence of endogenous compounds and the typically low concentrations of target analytes—needs efficient sample preparation strategies alongside high-performance instrumentation to achieve the sensitivity and selectivity required in modern analytical chemistry. In response to these challenges, recent advancements have focused on the development of advanced solid materials and their integration with sample preparation techniques. This review highlights recent progress in sorbents with enhanced selectivity, engineered materials such as crystalline frameworks, and the use of biopolymers as natural sorbents for drug analysis in biofluids. Additionally, the application of 3D-printed materials for the fabrication of extraction devices is presented. The article also provides insights into emerging trends and future directions in this evolving field.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100202"},"PeriodicalIF":6.5,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144749610","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 : 2025-08-01Epub Date: 2025-07-24DOI: 10.1016/j.sampre.2025.100203
Francesca Merlo, Andrea Speltini, Antonella Profumo
In the field of green sample preparation, new challenges are emerging for guaranteeing sustainability of analytical procedures and remarkable efforts have been made to develop materials from natural and/or renewable sources. In such a scenario, biochar is emerging as alternative sorbent with low economic and environmental impact. It is a carbon-rich material derived from the thermochemical conversion of biomass and waste and endowed with excellent textural properties such as high specific surface area and meso‑ and microporosity, and functional groups that are fundamental for the sorption behaviour, a key point in the analytical performance of biochar. These outstanding properties generated a growing interest in the use of biochar-based sorbents in sample preparation. In this context, this review provides an overview of the last 4-year applications of biochar in extraction techniques through an evaluation of greenness of the sample preparation procedures. At this purpose, two metric tools specific for the sample preparation, as AGREEprep and Sample Preparation Metric of Sustainability (SPMS), have been selected to give comprehensive evaluations about greenness, considering multiple criteria but with different weights and intervals in the parameters. Indeed, the papers here reviewed received in SPMS scores ranging from 5.16 to 10, and in AGREEprep from 0.16 to 0.7, evidencing there is space for improving extraction procedures involving biochar-based sorbents.
{"title":"Greenness of extraction procedures involving biochar-based sorbents for organic compounds","authors":"Francesca Merlo, Andrea Speltini, Antonella Profumo","doi":"10.1016/j.sampre.2025.100203","DOIUrl":"10.1016/j.sampre.2025.100203","url":null,"abstract":"<div><div>In the field of green sample preparation, new challenges are emerging for guaranteeing sustainability of analytical procedures and remarkable efforts have been made to develop materials from natural and/or renewable sources. In such a scenario, biochar is emerging as alternative sorbent with low economic and environmental impact. It is a carbon-rich material derived from the thermochemical conversion of biomass and waste and endowed with excellent textural properties such as high specific surface area and meso‑ and microporosity, and functional groups that are fundamental for the sorption behaviour, a key point in the analytical performance of biochar. These outstanding properties generated a growing interest in the use of biochar-based sorbents in sample preparation. In this context, this review provides an overview of the last 4-year applications of biochar in extraction techniques through an evaluation of greenness of the sample preparation procedures. At this purpose, two metric tools specific for the sample preparation, as AGREEprep and Sample Preparation Metric of Sustainability (SPMS), have been selected to give comprehensive evaluations about greenness, considering multiple criteria but with different weights and intervals in the parameters. Indeed, the papers here reviewed received in SPMS scores ranging from 5.16 to 10, and in AGREEprep from 0.16 to 0.7, evidencing there is space for improving extraction procedures involving biochar-based sorbents.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100203"},"PeriodicalIF":6.5,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144749611","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 : 2025-08-01Epub Date: 2025-05-22DOI: 10.1016/j.sampre.2025.100190
Christina Johannsen , Anna Kha Tu Nguyen , Sasha Shabani , Inger Oulie , Siri Dørum , Yvette Dehnes , Leon Reubsaet , Trine Grønhaug Halvorsen
Growth hormone-releasing hormone (GHRH) analogs, including sermorelin, CJC-1295, and tesamorelin, are prohibited in sports due to their performance-enhancing potential. Detecting these peptides remains challenging, requiring sensitive analytical techniques. This study explores the feasibility of dried serum spots (DSS) and smart samplers for detecting GHRH analogs in human serum using liquid chromatography-high-resolution tandem mass spectrometry. Smart samplers combine sampling and sample preparation in one tool; in this study smart samplers were developed using divinyl sulfone functionalized paper to immobilize antibodies for selective analyte capture. DSS and smart samplers were compared for extraction efficiency, precision, and detection capabilities. Various extraction approaches were evaluated to optimize analyte recovery followed by a blind sample study to assess detection capability at unknown concentrations. Results showed that DSS yielded higher overall signal intensities but exhibited greater variability. In contrast, smart samplers demonstrated improved reproducibility and sensitivity at lower concentrations. Smart samplers successfully identified sermorelin at 0.25 ng∙mL-1, CJC-1295 at 4 ng∙mL-1, and tesamorelin at 2.5 ng∙mL-1, while DSS exhibited limitations at these concentrations. This study presents a proof-of-concept for using smart samplers and DSS in anti-doping analysis. While the results shown are promising, further optimization is needed to improve analyte recovery and sampler stability. The findings support the potential of alternative blood sampling techniques in doping control and peptide biomarker analysis.
{"title":"Development of smart samplers and their comparison to dried serum spots for the analysis of growth hormone releasing hormone analogs using LCHRMS/MS","authors":"Christina Johannsen , Anna Kha Tu Nguyen , Sasha Shabani , Inger Oulie , Siri Dørum , Yvette Dehnes , Leon Reubsaet , Trine Grønhaug Halvorsen","doi":"10.1016/j.sampre.2025.100190","DOIUrl":"10.1016/j.sampre.2025.100190","url":null,"abstract":"<div><div>Growth hormone-releasing hormone (GHRH) analogs, including sermorelin, CJC-1295, and tesamorelin, are prohibited in sports due to their performance-enhancing potential. Detecting these peptides remains challenging, requiring sensitive analytical techniques. This study explores the feasibility of dried serum spots (DSS) and smart samplers for detecting GHRH analogs in human serum using liquid chromatography-high-resolution tandem mass spectrometry. Smart samplers combine sampling and sample preparation in one tool; in this study smart samplers were developed using divinyl sulfone functionalized paper to immobilize antibodies for selective analyte capture. DSS and smart samplers were compared for extraction efficiency, precision, and detection capabilities. Various extraction approaches were evaluated to optimize analyte recovery followed by a blind sample study to assess detection capability at unknown concentrations. Results showed that DSS yielded higher overall signal intensities but exhibited greater variability. In contrast, smart samplers demonstrated improved reproducibility and sensitivity at lower concentrations. Smart samplers successfully identified sermorelin at 0.25 ng∙mL<sup>-1</sup>, CJC-1295 at 4 ng∙mL<sup>-1</sup>, and tesamorelin at 2.5 ng∙mL<sup>-1</sup>, while DSS exhibited limitations at these concentrations. This study presents a proof-of-concept for using smart samplers and DSS in anti-doping analysis. While the results shown are promising, further optimization is needed to improve analyte recovery and sampler stability. The findings support the potential of alternative blood sampling techniques in doping control and peptide biomarker analysis.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100190"},"PeriodicalIF":5.2,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144185228","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 : 2025-08-01Epub Date: 2025-05-23DOI: 10.1016/j.sampre.2025.100191
Luana C. dos Santos , Juan Felipe Grisales-Mejía , Monique Martins Strieder , Jose A. Mendiola , Elena Ibáñez
Compressed fluids and novel green solvents represent the most promising approaches for achieving sustainable sample preparation in food analysis. Traditional extraction techniques often rely on toxic organic solvents and energy-intensive processes, leading to environmental concerns and inefficient workflows. Green Analytical Chemistry (GAC) promotes the adoption of eco-friendly alternatives that minimize solvent consumption, reduce waste, and enhance extraction efficiency. This review explores the role of compressed fluids’ technologies, including Pressurized Liquid Extraction (PLE), Supercritical Fluid Extraction (SFE), and Gas-Expanded Liquid Extraction (GXL) as viable replacements for conventional solvent-based methods. These techniques offer high selectivity, shorter extraction times, and lower environmental impact. Additionally, novel solvents such as deep eutectic solvents (DES), bio-based alternatives, and gas-expanded liquids present sustainable solutions that improve biodegradability, safety, and solvent recyclability. By integrating these innovative approaches into analytical workflows, food analysis can align with Green Chemistry principles while maintaining high analytical performance. This review critically evaluates the latest advancements in green sample preparation techniques based on pressurized fluids, highlighting their transformative potential in food safety, authenticity verification, and bioactive compound extraction.
{"title":"Innovative sample preparation techniques in food analysis: the rise of compressed fluids and novel solvents","authors":"Luana C. dos Santos , Juan Felipe Grisales-Mejía , Monique Martins Strieder , Jose A. Mendiola , Elena Ibáñez","doi":"10.1016/j.sampre.2025.100191","DOIUrl":"10.1016/j.sampre.2025.100191","url":null,"abstract":"<div><div>Compressed fluids and novel green solvents represent the most promising approaches for achieving sustainable sample preparation in food analysis. Traditional extraction techniques often rely on toxic organic solvents and energy-intensive processes, leading to environmental concerns and inefficient workflows. Green Analytical Chemistry (GAC) promotes the adoption of eco-friendly alternatives that minimize solvent consumption, reduce waste, and enhance extraction efficiency. This review explores the role of compressed fluids’ technologies, including Pressurized Liquid Extraction (PLE), Supercritical Fluid Extraction (SFE), and Gas-Expanded Liquid Extraction (GXL) as viable replacements for conventional solvent-based methods. These techniques offer high selectivity, shorter extraction times, and lower environmental impact. Additionally, novel solvents such as deep eutectic solvents (DES), bio-based alternatives, and gas-expanded liquids present sustainable solutions that improve biodegradability, safety, and solvent recyclability. By integrating these innovative approaches into analytical workflows, food analysis can align with Green Chemistry principles while maintaining high analytical performance. This review critically evaluates the latest advancements in green sample preparation techniques based on pressurized fluids, highlighting their transformative potential in food safety, authenticity verification, and bioactive compound extraction.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100191"},"PeriodicalIF":5.2,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144168993","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 : 2025-08-01Epub Date: 2025-07-11DOI: 10.1016/j.sampre.2025.100200
Hui Cao , WeiKang Guo , Ke Liu , Qin Shuai , Lijin Huang , Zhaochu Hu
Covalent organic frameworks (COFs) represent an emerging class of porous crystalline materials with immense potential as advanced materials for sample pretreatment. Their distinctive characteristics, including large specific surface areas, adjustable pore structures, robust chemical stability, and abundant active sites, render them a reliable platform for efficiently extracting analytes, thereby opening avenues for innovative applications in analytical chemistry. This review focuses on recent research progress in the utilization of functional COFs for the preconcentration of contaminants, including organic pollutants (such as drugs, pesticides, and dyes) and heavy metal ions. COFs featuring diverse functional groups, such as carboxyl, sulfonyl, hydroxyl, amino, nitro and halogen moieties and their integration with advanced sample pretreatment techniques are discussed. The review begins by examining two primary strategies for functionalizing COF: "bottom-up" and "post-synthetic modification". Subsequently, the interaction mechanisms and analytical performances of methods based on functionalized COFs are critically analyzed, emphasizing their extraction efficiency and selectivity. Finally, the technical merits of functional COFs as high-performance adsorbents in sample pretreatment are highlighted, while addressing current challenges and outlining future research directions. This review aims to provide a comprehensive reference for the rational design and practical applications of functionalized COFs in advanced sample pretreatment workflows.
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Pub Date : 2025-08-01Epub Date: 2025-07-07DOI: 10.1016/j.sampre.2025.100198
Rui Zhang , Ren-Jie Yang , Ping-An Zhang , Shao-Ting Wang
Background
Precise measurement of immunosuppressant levels in whole blood is critical for monitoring post-transplant patient outcomes. Conventional protein precipitation (PP) methods, which rely on vortex mixing and centrifugation, present substantial limitations in terms of automation and scalability. To address these challenges, we developed a novel pretreatment strategy termed “Pseudo-Protein-Precipitation combined with Cold-Induced Phase Separation” (PPP+CIPS), designed to simplify sample processing and enhance high-throughput efficiency.
Results
The PPP+CIPS method employs 48 % acetonitrile to generate a semi-homogeneous blood suspension, enabling in-situ drug extraction via CIPS. Notably, this approach eliminates the need for vortexing and centrifugation—key bottlenecks in traditional therapeutic drug monitoring workflows. By leveraging 96-well plates and multi-channel pipettes, the protocol reduces pretreatment time to approximately one-third of that required by PP. Clinical validation (n = 288 in total) revealed strong concordance with established methods, with 94 % of tacrolimus, 95 % of cyclosporin A, and 92 % of sirolimus measurements falling within ±20 % agreement limits.
Significance
The PPP+CIPS strategy marks a significant leap forward in high-throughput therapeutic drug monitoring for immunosuppressants. Its seamless integration with 96-well formats and static processing workflows makes it a promising cornerstone for future automated and integrated TDM systems.
{"title":"Pretreat immunosuppressants in whole blood without vortexing and centrifugation","authors":"Rui Zhang , Ren-Jie Yang , Ping-An Zhang , Shao-Ting Wang","doi":"10.1016/j.sampre.2025.100198","DOIUrl":"10.1016/j.sampre.2025.100198","url":null,"abstract":"<div><h3>Background</h3><div>Precise measurement of immunosuppressant levels in whole blood is critical for monitoring post-transplant patient outcomes. Conventional protein precipitation (PP) methods, which rely on vortex mixing and centrifugation, present substantial limitations in terms of automation and scalability. To address these challenges, we developed a novel pretreatment strategy termed “Pseudo-Protein-Precipitation combined with Cold-Induced Phase Separation” (PPP+CIPS), designed to simplify sample processing and enhance high-throughput efficiency.</div></div><div><h3>Results</h3><div>The PPP+CIPS method employs 48 % acetonitrile to generate a semi-homogeneous blood suspension, enabling in-situ drug extraction via CIPS. Notably, this approach eliminates the need for vortexing and centrifugation—key bottlenecks in traditional therapeutic drug monitoring workflows. By leveraging 96-well plates and multi-channel pipettes, the protocol reduces pretreatment time to approximately one-third of that required by PP. Clinical validation (<em>n</em> = 288 in total) revealed strong concordance with established methods, with 94 % of tacrolimus, 95 % of cyclosporin A, and 92 % of sirolimus measurements falling within ±20 % agreement limits.</div></div><div><h3>Significance</h3><div>The PPP+CIPS strategy marks a significant leap forward in high-throughput therapeutic drug monitoring for immunosuppressants. Its seamless integration with 96-well formats and static processing workflows makes it a promising cornerstone for future automated and integrated TDM systems.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100198"},"PeriodicalIF":5.2,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144595951","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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