Pub 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":"2025-08-20","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 : 2025-08-01DOI: 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 : 2025-08-01DOI: 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 : 2025-08-01DOI: 10.1016/j.sampre.2025.100209
Maedeh Saadat, Yadollah Yamini
Antifungals drugs are widely used for variety of fungal infections. Extraction and determination of these drugs in biological sample is crucial because of their toxicity, endocrine-disrupting, and cytochrome P450-mediated effects. In addition, developing an efficient and stable sorbent with a high surface area for microextraction by packed sorbent (MEPS) technique is of great interest. Triple-shell Co/Ni-based hydroxide phosphate (TS-CNHP) was synthesized for increasing surface area. For characterization of TS-CNHP, a combination of advanced analytical methods was employed. Field-emission scanning electron microscopy, transmission electron microscopy, Fourier-transform infrared spectroscopy, Brunauer–Emmett–Teller, dynamic light scattering and X-ray diffraction. In this work the MEPS was coupled with high-performance liquid chromatography equipped with an ultraviolet detector (HPLC-UV). The TS-CNHP demonstrated an impressive level of efficiency and the selectivity for the adsorption of azole antifungals. The optimal conditions for MEPS were determined through a systematic evaluation of key parameters influencing analyte extraction efficiency. These parameters included: pH (6), adsorption time (7 min), adsorption cycles (2 cycles), salt addition (0%), elution solvent (methanol), desorption flow rate (100 µL min-1), desorption volume (400 µL), and desorption cycles (2 cycles). The analytical performance of the method was thoroughly assessed under optimized conditions. The relative standard deviations (RSDs) ranged from 2.7% to 5.4%, demonstrating a high level of precision. Furthermore, extraction recoveries were observed between 78.0% and 89.7%. A wide linear dynamic range (0.5–1000 μg l-1) and an acceptable LOD (0.2 µg L−1) for all of the analytes were achieved. The coefficients of determination (R2) of ketoconazole, clotrimazole and miconazole are 0.9985, 0.9986 and 0.9989 respectively, which demonstrating the reliability of the method The proposed MEPS-HPLC-UV technique demonstrates remarkable analytical efficiency in the extraction and quantification of trace levels of azole antifungals from biological matrices, specifically dog and human hair.
抗真菌药物广泛用于各种真菌感染。由于这些药物的毒性、内分泌干扰和细胞色素p450介导的作用，在生物样品中提取和测定这些药物至关重要。此外，利用填充吸附剂（MEPS）技术开发一种高效、稳定、高表面积的微萃取吸附剂也具有重要意义。合成了三壳层Co/ ni基氢氧化磷（TS-CNHP），以增加比表面积。为了表征TS-CNHP，结合了先进的分析方法。场发射扫描电子显微镜，透射电子显微镜，傅里叶变换红外光谱，布鲁诺尔-埃米特-泰勒，动态光散射和x射线衍射。在这项工作中，MEPS与配备紫外检测器的高效液相色谱（HPLC-UV）相结合。TS-CNHP表现出了令人印象深刻的效率和选择性吸附唑类抗真菌物质。通过对影响分析物萃取效率的关键参数进行系统评价，确定了MEPS萃取的最佳工艺条件。这些参数包括：pH(6)、吸附时间（7 min）、吸附次数（2次）、加盐量（0%）、洗脱溶剂（甲醇）、解吸流量（100µL min-1）、解吸体积（400µL）、解吸次数（2次）。在优化条件下，对该方法的分析性能进行了全面评价。相对标准偏差（rsd）范围为2.7% ~ 5.4%，具有较高的精度。提取回收率在78.0% ~ 89.7%之间。所有分析物具有宽的线性动态范围（0.5-1000 μg L -1）和可接受的LOD （0.2 μg L -1）。酮康唑、克霉唑和咪康唑的测定系数（R2）分别为0.9985、0.9986和0.9989，证明了该方法的可靠性。MEPS-HPLC-UV技术在提取和定量生物基质（特别是犬和人毛发）中痕量唑类抗真菌药物方面具有良好的分析效率。
{"title":"Multiple-shell amorphous Co/Ni-(PO4)x(OH)y hollow layered double hydroxide for enhanced extraction of some azole antifungals from biological samples","authors":"Maedeh Saadat, Yadollah Yamini","doi":"10.1016/j.sampre.2025.100209","DOIUrl":"10.1016/j.sampre.2025.100209","url":null,"abstract":"<div><div>Antifungals drugs are widely used for variety of fungal infections. Extraction and determination of these drugs in biological sample is crucial because of their toxicity, endocrine-disrupting, and cytochrome P450-mediated effects. In addition, developing an efficient and stable sorbent with a high surface area for microextraction by packed sorbent (MEPS) technique is of great interest. Triple-shell Co/Ni-based hydroxide phosphate (TS-CNHP) was synthesized for increasing surface area. For characterization of TS-CNHP, a combination of advanced analytical methods was employed. Field-emission scanning electron microscopy, transmission electron microscopy, Fourier-transform infrared spectroscopy, Brunauer–Emmett–Teller, dynamic light scattering and X-ray diffraction. In this work the MEPS was coupled with high-performance liquid chromatography equipped with an ultraviolet detector (HPLC-UV). The TS-CNHP demonstrated an impressive level of efficiency and the selectivity for the adsorption of azole antifungals. The optimal conditions for MEPS were determined through a systematic evaluation of key parameters influencing analyte extraction efficiency. These parameters included: pH (6), adsorption time (7 min), adsorption cycles (2 cycles), salt addition (0%), elution solvent (methanol), desorption flow rate (100 µL min<sup>-1</sup>), desorption volume (400 µL), and desorption cycles (2 cycles). The analytical performance of the method was thoroughly assessed under optimized conditions. The relative standard deviations (RSDs) ranged from 2.7% to 5.4%, demonstrating a high level of precision. Furthermore, extraction recoveries were observed between 78.0% and 89.7%. A wide linear dynamic range (0.5–1000 μg l<sup>-1</sup>) and an acceptable LOD (0.2 µg L<sup>−1</sup>) for all of the analytes were achieved. The coefficients of determination (R<sup>2</sup>) of ketoconazole, clotrimazole and miconazole are 0.9985, 0.9986 and 0.9989 respectively, which demonstrating the reliability of the method The proposed MEPS-HPLC-UV technique demonstrates remarkable analytical efficiency in the extraction and quantification of trace levels of azole antifungals from biological matrices, specifically dog and human hair.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100209"},"PeriodicalIF":6.5,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144925091","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 : 2025-08-01DOI: 10.1016/j.sampre.2025.100208
Jiarui Zhang , Shuang Feng , Yalin Xi , Meiyun Shi , Lei Yin
Magnetic nanomaterials (MNMs) are highly effective sorbents for biomedical sample pretreatment, leveraging their superparamagnetism, large specific surface area, and tunable surface functionalities. This review comprehensively examines MNM classification, synthesis techniques, and functionalization approaches, highlighting their pivotal role in magnetic solid-phase extraction (MSPE) for analyte enrichment. We systematically detail MNM applications in biomedical sample processing, focusing on MSPE for efficient nucleotide isolation, specific protein capture, and ultrasensitive biomarker detection. While MNM-based MSPE offers significant advantages in sensitivity, selectivity, and operational simplicity, challenges remain in achieving reproducible synthesis and deepening the mechanistic understanding of adsorption processes. Future research should prioritize developing automated MSPE platforms and multifunctional MNMs capable of addressing complex clinical matrices. This work provides a valuable reference for designing next-generation analytical systems utilizing MNMs.
{"title":"Advances in magnetic nanomaterials for biomedical sample pretreatment: synthesis, functionalization, and applications in magnetic solid-phase extraction","authors":"Jiarui Zhang , Shuang Feng , Yalin Xi , Meiyun Shi , Lei Yin","doi":"10.1016/j.sampre.2025.100208","DOIUrl":"10.1016/j.sampre.2025.100208","url":null,"abstract":"<div><div>Magnetic nanomaterials (MNMs) are highly effective sorbents for biomedical sample pretreatment, leveraging their superparamagnetism, large specific surface area, and tunable surface functionalities. This review comprehensively examines MNM classification, synthesis techniques, and functionalization approaches, highlighting their pivotal role in magnetic solid-phase extraction (MSPE) for analyte enrichment. We systematically detail MNM applications in biomedical sample processing, focusing on MSPE for efficient nucleotide isolation, specific protein capture, and ultrasensitive biomarker detection. While MNM-based MSPE offers significant advantages in sensitivity, selectivity, and operational simplicity, challenges remain in achieving reproducible synthesis and deepening the mechanistic understanding of adsorption processes. Future research should prioritize developing automated MSPE platforms and multifunctional MNMs capable of addressing complex clinical matrices. This work provides a valuable reference for designing next-generation analytical systems utilizing MNMs.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100208"},"PeriodicalIF":6.5,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144903830","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}
The development of novel membranes through green chemistry remains a significant challenge in advancing practical separation science. In this study, a sodium alginate-g-polyacrylic acid/agarose hydrogel was synthesized and, for the first time, applied as a membrane in gel electromembrane extraction (G-EME) for the isolation of morphine, a basic analyte, from urine samples. The extracted morphine was subsequently quantified using differential pulse voltammetry (DPV) with a glassy carbon electrode. The hydrogel membrane (5 mm thick) was prepared using 0.75 % (w/v) sodium alginate, 3.80 % (v/v) acrylic acid, 0.04 % (w/v) ammonium persulfate, and 1.25 % (w/v) agarose. The extraction process was optimized by evaluating factors such as membrane composition, extraction time, applied voltage, and pHs of the sample solution, membrane, and acceptor phase (AP). Under optimal conditions (25 min extraction time, 70 V applied voltage, membrane pH 4.0, AP pH 3.0, and sample solution pH 7.0) morphine was efficiently extracted through the hydrogel membrane and transferred to an aqueous AP. The collected AP was mixed with 0.15 M phosphate buffer (pH 7.0) and analyzed voltammetrically. The method achieved a limit of detection of 0.09 μg/mL and a limit of quantification of 0.28 μg/mL, and was successfully applied for morphine determination in urine sample. The polyacrylic acid-based membrane enhanced extraction efficiency through electrostatic interactions, while the use of DPV offered clearer signal interpretation and reduced background current, facilitating reliable detection of trace analytes. These advantages support the method’s potential for simple, selective, and environmentally friendly analysis of basic drugs in biological samples.
{"title":"A green approach for electromembrane extraction of morphine from urine using sodium alginate-g-polyacrylic acid/agarose hydrogel membrane","authors":"Elnaz Khodabakhshi , Somayeh Makarem , Mehran Kurdtabar , Saeed Nojavan","doi":"10.1016/j.sampre.2025.100204","DOIUrl":"10.1016/j.sampre.2025.100204","url":null,"abstract":"<div><div>The development of novel membranes through green chemistry remains a significant challenge in advancing practical separation science. In this study, a sodium alginate-g-polyacrylic acid/agarose hydrogel was synthesized and, for the first time, applied as a membrane in gel electromembrane extraction (G-EME) for the isolation of morphine, a basic analyte, from urine samples. The extracted morphine was subsequently quantified using differential pulse voltammetry (DPV) with a glassy carbon electrode. The hydrogel membrane (5 mm thick) was prepared using 0.75 % (w/v) sodium alginate, 3.80 % (v/v) acrylic acid, 0.04 % (w/v) ammonium persulfate, and 1.25 % (w/v) agarose. The extraction process was optimized by evaluating factors such as membrane composition, extraction time, applied voltage, and pHs of the sample solution, membrane, and acceptor phase (AP). Under optimal conditions (25 min extraction time, 70 V applied voltage, membrane pH 4.0, AP pH 3.0, and sample solution pH 7.0) morphine was efficiently extracted through the hydrogel membrane and transferred to an aqueous AP. The collected AP was mixed with 0.15 M phosphate buffer (pH 7.0) and analyzed voltammetrically. The method achieved a limit of detection of 0.09 μg/mL and a limit of quantification of 0.28 μg/mL, and was successfully applied for morphine determination in urine sample. The polyacrylic acid-based membrane enhanced extraction efficiency through electrostatic interactions, while the use of DPV offered clearer signal interpretation and reduced background current, facilitating reliable detection of trace analytes. These advantages support the method’s potential for simple, selective, and environmentally friendly analysis of basic drugs in biological samples.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100204"},"PeriodicalIF":6.5,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144780679","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 : 2025-08-01DOI: 10.1016/j.sampre.2025.100205
Miryam Perrucci , Erika Maria Ricci , Abuzar Kabir , Kenneth G. Furton , Marcello Locatelli
To minimize the environmental and human health impacts of chemical processes, there is growing interest in eco-friendly methods aligned with the principles of Green Analytical Chemistry (GAC). A successful chemical analysis typically involves sample preparation, sampling, separation and analysis, quantification, and data interpretation. Among these, sample preparation plays a crucial role in isolating and preconcentrating target analytes from complex matrices.
In 2014, fabric phase sorptive extraction (FPSE) was introduced as a simplified and greener sample pretreatment method. Building on this advancement and a recent patent, the present study introduces an innovative 3D-printed device designed for use with a range of target analytes and complex sample matrices. Constructed from inert materials, the device features a rigid, modular structure with multiple windows that securely hold various membrane-based extraction materials. These include FPSE membranes, electrospun membranes, and materials derived from adsorbent systems recovered from production or usage waste, as well as permeable molecularly imprinted polymers (MIPs).
The device offers several advantages, including enhanced enrichment factors, compatibility with diverse planar membrane types, and highly customizable selectivity based on membrane configuration and chemistry. Its design also incorporates a built-in slot for a magnetic stirrer, enabling precise control of rotation speed during extraction-even in field conditions using a portable, battery-powered stirrer.
Experimental results unequivocally demonstrate that the new device achieves superior enrichment factors compared to previously validated methods for the same analytes, confirming its effectiveness and potential for broader analytical applications.
{"title":"3D-printed device for improved membrane-based extraction procedure of xenobiotics in complex matrices","authors":"Miryam Perrucci , Erika Maria Ricci , Abuzar Kabir , Kenneth G. Furton , Marcello Locatelli","doi":"10.1016/j.sampre.2025.100205","DOIUrl":"10.1016/j.sampre.2025.100205","url":null,"abstract":"<div><div>To minimize the environmental and human health impacts of chemical processes, there is growing interest in eco-friendly methods aligned with the principles of Green Analytical Chemistry (GAC). A successful chemical analysis typically involves sample preparation, sampling, separation and analysis, quantification, and data interpretation. Among these, sample preparation plays a crucial role in isolating and preconcentrating target analytes from complex matrices.</div><div>In 2014, fabric phase sorptive extraction (FPSE) was introduced as a simplified and greener sample pretreatment method. Building on this advancement and a recent patent, the present study introduces an innovative 3D-printed device designed for use with a range of target analytes and complex sample matrices. Constructed from inert materials, the device features a rigid, modular structure with multiple windows that securely hold various membrane-based extraction materials. These include FPSE membranes, electrospun membranes, and materials derived from adsorbent systems recovered from production or usage waste, as well as permeable molecularly imprinted polymers (MIPs).</div><div>The device offers several advantages, including enhanced enrichment factors, compatibility with diverse planar membrane types, and highly customizable selectivity based on membrane configuration and chemistry. Its design also incorporates a built-in slot for a magnetic stirrer, enabling precise control of rotation speed during extraction-even <em>in field</em> conditions using a portable, battery-powered stirrer.</div><div>Experimental results unequivocally demonstrate that the new device achieves superior enrichment factors compared to previously validated methods for the same analytes, confirming its effectiveness and potential for broader analytical applications.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100205"},"PeriodicalIF":6.5,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144780678","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 : 2025-07-17DOI: 10.1016/j.sampre.2025.100201
Miguel Ángel Aguirre , Natalia Arroyo-Manzanares , Laura Carbonell-Rozas , José Grau , Carlos Moreno , Lorena Vidal
The miniaturization of conventional extraction techniques, particularly microextraction methods, has led to a reduction in the use of hazardous reagents and waste. However, the continued use of toxic solvents and materials, along with time-consuming sample preparation processes, negatively impacts the overall sustainability of these methods. As a result, there is growing interest in exploring greener alternatives. This review highlights the most promising green solvents for liquid-phase microextraction, including (natural) deep eutectic solvents, low-toxicity ionic liquids, surfactants, micellar solvents, and bio-based solvents, emphasizing their applications in innovative sample preparation techniques in the last five years. Particular emphasis is placed on their use in automated and semi-automated systems, in line with the increasing role of automation in Analytical Chemistry. Selected applications have been carefully reviewed and discussed to illustrate key advances in the use of green solvents and automation for extracting a wide range of compounds from various matrices. In addition, future perspectives are outlined to guide further development of liquid-phase microextraction in alignment with current trends in green sample preparation.
{"title":"Recent green approaches in liquid-phase microextraction","authors":"Miguel Ángel Aguirre , Natalia Arroyo-Manzanares , Laura Carbonell-Rozas , José Grau , Carlos Moreno , Lorena Vidal","doi":"10.1016/j.sampre.2025.100201","DOIUrl":"10.1016/j.sampre.2025.100201","url":null,"abstract":"<div><div>The miniaturization of conventional extraction techniques, particularly microextraction methods, has led to a reduction in the use of hazardous reagents and waste. However, the continued use of toxic solvents and materials, along with time-consuming sample preparation processes, negatively impacts the overall sustainability of these methods. As a result, there is growing interest in exploring greener alternatives. This review highlights the most promising green solvents for liquid-phase microextraction, including (natural) deep eutectic solvents, low-toxicity ionic liquids, surfactants, micellar solvents, and bio-based solvents, emphasizing their applications in innovative sample preparation techniques in the last five years. Particular emphasis is placed on their use in automated and semi-automated systems, in line with the increasing role of automation in Analytical Chemistry. Selected applications have been carefully reviewed and discussed to illustrate key advances in the use of green solvents and automation for extracting a wide range of compounds from various matrices. In addition, future perspectives are outlined to guide further development of liquid-phase microextraction in alignment with current trends in green sample preparation.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100201"},"PeriodicalIF":5.2,"publicationDate":"2025-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144685863","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 : 2025-07-11DOI: 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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A 3D-printed handheld device has been developed for rapid and efficient sample preparation, extracting pathogen total nucleic acids from citrus leaves for downstream molecular analysis. With its high-speed motor, knurled lysis chamber for rapid sample lysis, and quick nucleic acid extraction using cellulose paper disks (Whatman CHR1), this device can yield ready-to-use DNA and RNA in just 12 min. All components, except for the motor, wiring, and paper disks, were printed in-house using a PolyJet 3D printer with photosensitive resins. The device was optimized for maximum sample lysis by evaluating operation voltages and chamber features, as measured by DNA and RNA concentrations using a Qubit fluorometer and quantification cycle (Cq) values obtained through qPCR assays. The results showed that the lysis chamber with internal knurling and the motor operated at 7.5 V was sufficient for effective sample lysis in 1 min, achieving RNA concentrations up to 87.6 % of those obtained with mortar-and-pestle grinding. Paper disk washing and elution conditions were also optimized using a NanoDrop spectrophotometer and qPCR assays, where two 1-minute washes and a 100 µL elution volume resulted in the highest purity and lowest Cq value. The optimized handheld device was validated with citrus sources infected with Citrus tristeza virus (CTV) and Spiroplasma citri (S. citri), demonstrating high detection accuracy (100 %) and low assay variation (CV < 3.8 %) in qPCR-based analysis. Based on these successful results, this device is expected to be broadly applicable to similar viral and bacterial pathogens affecting plants.
{"title":"A 3D-printed handheld device for quick citrus tissue lysis and nucleic acid extraction","authors":"Chia-Wei Liu , Brent Kalish , Sohrab Bodaghi , Georgios Vidalakis , Hideaki Tsutsui","doi":"10.1016/j.sampre.2025.100199","DOIUrl":"10.1016/j.sampre.2025.100199","url":null,"abstract":"<div><div>A 3D-printed handheld device has been developed for rapid and efficient sample preparation, extracting pathogen total nucleic acids from citrus leaves for downstream molecular analysis. With its high-speed motor, knurled lysis chamber for rapid sample lysis, and quick nucleic acid extraction using cellulose paper disks (Whatman CHR1), this device can yield ready-to-use DNA and RNA in just 12 min. All components, except for the motor, wiring, and paper disks, were printed in-house using a PolyJet 3D printer with photosensitive resins. The device was optimized for maximum sample lysis by evaluating operation voltages and chamber features, as measured by DNA and RNA concentrations using a Qubit fluorometer and quantification cycle (Cq) values obtained through qPCR assays. The results showed that the lysis chamber with internal knurling and the motor operated at 7.5 V was sufficient for effective sample lysis in 1 min, achieving RNA concentrations up to 87.6 % of those obtained with mortar-and-pestle grinding. Paper disk washing and elution conditions were also optimized using a NanoDrop spectrophotometer and qPCR assays, where two 1-minute washes and a 100 µL elution volume resulted in the highest purity and lowest Cq value. The optimized handheld device was validated with citrus sources infected with <em>Citrus tristeza virus</em> (CTV) and <em>Spiroplasma citri</em> (<em>S. citri</em>), demonstrating high detection accuracy (100 %) and low assay variation (CV < 3.8 %) in qPCR-based analysis. Based on these successful results, this device is expected to be broadly applicable to similar viral and bacterial pathogens affecting plants.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100199"},"PeriodicalIF":5.2,"publicationDate":"2025-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144634324","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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