P. García-Atienza, A. García-Juan, S. Armenta, J.M. Herrero-Martínez, H. Martínez-Pérez-Cejuela
{"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}
Francesca Merlo, Andrea Speltini, Antonella Profumo
{"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}
Miguel Ángel Aguirre , Natalia Arroyo-Manzanares , Laura Carbonell-Rozas , José Grau , Carlos Moreno , Lorena Vidal
{"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}
Hui Cao , WeiKang Guo , Ke Liu , Qin Shuai , Lijin Huang , Zhaochu Hu
{"title":"Progress in functional covalent organic frameworks as advanced materials for sample pretreatment","authors":"Hui Cao , WeiKang Guo , Ke Liu , Qin Shuai , Lijin Huang , Zhaochu Hu","doi":"10.1016/j.sampre.2025.100200","DOIUrl":"10.1016/j.sampre.2025.100200","url":null,"abstract":"<div><div>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.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100200"},"PeriodicalIF":5.2,"publicationDate":"2025-07-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144663689","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}
{"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}
Rui Zhang , Ren-Jie Yang , Ping-An Zhang , Shao-Ting Wang
{"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":"2025-07-07","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}
{"title":"Supported liquid membrane-coupled Extraction","authors":"Shengjie Hu , Xiantao Shen , Chuixiu Huang","doi":"10.1016/j.sampre.2025.100197","DOIUrl":"10.1016/j.sampre.2025.100197","url":null,"abstract":"<div><div>Group separation of multiple analytes with diverse physicochemical properties from the same complex sample is significant in clinical diagnosis, environmental monitoring and biomarker identification. To achieve this goal, supported liquid membrane (SLM)-coupled extraction techniques were developed by integrating two or more SLM-based extraction processes, either simultaneously or sequentially. This approach offers several advantages such as low sample consumption, short operational time, and efficient group separation. In recent years, SLM-coupled extraction approaches have been successfully applied to extract multiple targets from complex biological samples and environmental samples. However, the reviews in the literature mainly focused on a single SLM extraction technique, either liquid-phase microextraction (LPME) or electromembrane extraction (EME). Therefore, a comprehensive overview of SLM-coupled extraction techniques is still lack. The current review comprehensively summarizes the advances in SLM-coupled extraction techniques. We elaborate three types of SLM-coupled extraction techniques, including coupled-LPME, coupled-EME and EME/LPME. Moreover, a prospective discussion on the future development trends of the SLM-coupled extraction techniques is also provided.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100197"},"PeriodicalIF":5.2,"publicationDate":"2025-07-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144632451","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}
{"title":"Enhanced electromembrane extraction of acidic drugs using a chitosan-agarose hybrid gel membrane","authors":"Hasti Gharah Sheikhlou , Majid Gharah Sheikhlou , Marzieh Saberi , Saeed Nojavan","doi":"10.1016/j.sampre.2025.100196","DOIUrl":"10.1016/j.sampre.2025.100196","url":null,"abstract":"<div><div>In this study, a novel chitosan-agarose gel membrane was developed and applied in the gel electromembrane extraction (G-EME) technique to extract and preconcentrate two model acidic drugs, naproxen and ibuprofen, from urine samples. Chitosan, acting as a positively charged agent and viscosifier, significantly improved extraction efficiency by reducing electric current and minimizing the electroendosmosis (EEO) effect. The parameters affecting the extraction recoveries were optimized and evaluated using both one-variable-at-a-time and Box–Behnken design approaches alongside response surface methodology. To maximize drugs recovery from a 7.0 mL urine sample, the following parameters were optimized: a membrane composed of 3.0 % (w/v) agarose and 1.0 % (w/v) chitosan, pH of the gel membrane: 5.5, extraction voltage: 32.5 V, pH of the donor phase: 8.0, pH of the acceptor phase: 11.0, extraction time: 21 min, volume of acceptor phase: 200 µL, gel membrane thickness: ∼ 4 mm and donor phase stirring speed: 500 rpm. Under optimal conditions, the extraction recoveries were 60.4 % for naproxen and 81.9 % for ibuprofen. Limits of detection for naproxen and ibuprofen were 3.0 and 4.5 ng/mL, respectively. This method was successfully applied to quantify acidic drugs in real urine samples, achieving relative recoveries in the range of 91.2–94.9 %, demonstrating excellent reliability for biological matrices.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100196"},"PeriodicalIF":5.2,"publicationDate":"2025-06-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144570583","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}
{"title":"Evaluation of performance and matrix compatibility of mixed mode C18-SCX SPME fibers for compounds with different physicochemical properties","authors":"Marcos Tascon , Ezel Boyaci , Nathaly Reyes-Garcés , Janusz Pawliszyn","doi":"10.1016/j.sampre.2025.100195","DOIUrl":"10.1016/j.sampre.2025.100195","url":null,"abstract":"<div><div>Solid-phase microextraction (SPME) has evolved significantly since its inception, yet challenges remain in developing coatings fully compatible with LC-MS that combine broad polarity coverage with biocompatibility for complex matrices. This study evaluates mixed-mode C<sub>18</sub>-SCX (strong cation exchange) SPME fibers designed to extract analytes of a wide range of physicochemical properties, addressing limitations in current methodologies. The fibers were tested for extraction efficiency, reproducibility, and matrix compatibility using a group of model compounds with different physicochemical properties, namely, codeine (logP=1.19), carbamazepine (logP=2.45), diazepam (logP=2.82), and propranolol (logP=3.47). Furthermore, the biocompatibility was tested in diverse matrices, such as PBS, blood, plasma, urine, and grape juice.</div><div>Results demonstrated exceptional inter-fiber reproducibility (RSD ≤ 15 %, <em>n</em> = 96 fibers) and robust performance in biomatrices, with relative matrix effects primarily governed by analyte binding affinities to matrix macromolecules rather than coating fouling. Absolute matrix effects were negligible (93–111 %), underscoring the fibers’ ability to deliver clean extracts for LC-MS analysis. Fiber reusability was validated over three consecutive extractions (RSD ≤ 10 %), and morphological integrity was preserved post-extraction, even in challenging matrices like whole blood. This work represents the versatility of mixed-mode SPME fibers for high-throughput bioanalysis, offering a significant advancement for in vivo and in vitro targeted and untargeted applications.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100195"},"PeriodicalIF":5.2,"publicationDate":"2025-06-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144549565","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}
Madison E. Walbrun , Aamna Aijaz , Gabriella Ryan , John D. Bunting , Zachary P. Morehouse , Rodney J. Nash
{"title":"Improved sample preparation using bead mill homogenization","authors":"Madison E. Walbrun , Aamna Aijaz , Gabriella Ryan , John D. Bunting , Zachary P. Morehouse , Rodney J. Nash","doi":"10.1016/j.sampre.2025.100194","DOIUrl":"10.1016/j.sampre.2025.100194","url":null,"abstract":"<div><div>Proper sample preparation is the key to having successful data analysis downstream. Despite the many efforts to improve sample preparation, there are still many inconsistencies and challenges when attempting to produce a sample for downstream analysis. Here we compare common methods used in sample preparation (detergent and manual Dounce homogenization) to mechanical Bead Mill homogenization. These methods have been shown to lyse both cell and tissue, however, concentrations and detectability of desired analytes can be greatly reduced. These results show that mechanical Bead Mill homogenization requires less starting sample, and less time, while producing higher protein concentrations with increased reproducibility, therefore improving downstream analysis.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100194"},"PeriodicalIF":5.2,"publicationDate":"2025-06-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144556795","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}