Mussab Uddin , Faizah Mohammad Yunus , Zaharaddeen Muhammad , Muggundha Raoov , Andrew William King , Waleed Alahmad , Sibel A. Ozkan
{"title":"Advances in microextraction techniques utilizing deep eutectic solvents for the extraction of antibiotics","authors":"Mussab Uddin , Faizah Mohammad Yunus , Zaharaddeen Muhammad , Muggundha Raoov , Andrew William King , Waleed Alahmad , Sibel A. Ozkan","doi":"10.1016/j.sampre.2025.100172","DOIUrl":"10.1016/j.sampre.2025.100172","url":null,"abstract":"<div><div>The emergence of antibiotic contamination in food, water, and environmental matrices has necessitated the development of efficient, sensitive, and environmentally sustainable analytical methods. Deep eutectic solvents (DESs) have attracted significant attention as green alternatives to conventional solvents owing to their tunable properties, low toxicity, and biodegradability. This review comprehensively explores recent advancements in DES-based microextraction techniques for antibiotic detection, including solid-phase microextraction, liquid-liquid microextraction, and vortex-assisted approaches. Integration with cutting-edge analytical instruments, such as high-performance liquid chromatography with mass spectrometry and ion-mobility spectrometry, has enhanced the selectivity and sensitivity of trace-level antibiotics.</div><div>Key challenges, such as DES viscosity and scalability, were critically examined alongside emerging solutions, including novel DES formulations and functional additives for improved extraction efficiency. This review underscores the role of DES-based microextraction in facilitating greener analytical practices, and highlights its potential for broader applications in environmental monitoring, pharmaceutical residue analysis, and food safety. By identifying the current limitations and offering strategies for future research, this review provides a valuable resource for advancing sustainable antibiotic extraction approaches.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100172"},"PeriodicalIF":5.2,"publicationDate":"2025-03-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143577967","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Recent advances in environmental sample preparation: Nanomaterials, automation, and sustainable strategies","authors":"Federico Belén , Julián Gutiérrez , Valeria Springer","doi":"10.1016/j.sampre.2025.100171","DOIUrl":"10.1016/j.sampre.2025.100171","url":null,"abstract":"<div><div>The increasing occurrence of micropollutants and the need for their monitoring in environmental matrices have driven the demand for more efficient and accurate analytical methods. In particular, sample preparation procedures are essential for addressing the complexity of environmental samples while ensuring high sensitivity. To meet these demands, various nanomaterials (NMs) have been proposed as extractive phases for development of miniaturized sorbent-based extraction approaches. These NMs, ranging from carbon-based nanostructures and metal-based or metal oxide nanoparticles, to metal–organic composites, are at the forefront of innovation due to their exceptional surface areas, tunable properties, ease of functionalization and, in some cases, green production routes. On the other hand, the development of (semi)automated platforms has facilitated high-throughput and reproducible sample processing, significantly reducing the use of reagents, time, and labor. This review highlights the pivotal role of NMs and automation in advancing sample preparation methodologies over the past five years, in alignment with green sample preparation (GSP) guidelines. Additionally, the integration of emerging technologies, such as 3D printing, is discussed in the context of developing modern sample preparation methods. Recent contributions involving miniaturized platforms, green nanosorbents, and the integration of processing steps with automation, are evaluated for their potential to provide highly efficient, cost-effective solutions for monitoring micropollutants in environmental matrices.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100171"},"PeriodicalIF":5.2,"publicationDate":"2025-03-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143619453","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Samira Dowlatshah , Anne Oldeide Hay , Line Noreng , Frederik André Hansen
{"title":"A practical tutorial for optimizing electromembrane extraction methods by response surface methodology","authors":"Samira Dowlatshah , Anne Oldeide Hay , Line Noreng , Frederik André Hansen","doi":"10.1016/j.sampre.2025.100170","DOIUrl":"10.1016/j.sampre.2025.100170","url":null,"abstract":"<div><div>Microextraction techniques, such as electromembrane extraction (EME), have greatly advanced analytical chemistry by providing efficient, cost-effective, and eco-friendly sample preparation methods. EME is especially promising for ionizable analytes, with its success relying on optimizing multiple experimental variables. Traditionally, optimization has employed a one-variable-at-a-time (OVAT) approach, which is time-consuming and may overlooks variable interactions. This tutorial introduces response surface methodology (RSM) as a superior alternative for optimizing EME methods. RSM allows for the simultaneous variation of multiple factors, offering a comprehensive understanding of their effects and interactions with fewer experiments. This tutorial covers the fundamental principles of EME, essential experimental parameters, and the application of RSM for method optimization. It includes guidance on software selection, design choice, factor settings, response definition, and the optimization of multiple responses. Practical steps for conducting experiments, analyzing data, and interpreting models are detailed, with real-life examples illustrating the process. The tutorial aims to make RSM accessible to both novice and moderately experienced users, promoting its broader application in analytical chemistry. By simplifying the complex optimization process, this tutorial supports the development of robust, efficient, and green EME methods.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100170"},"PeriodicalIF":5.2,"publicationDate":"2025-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143578038","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Nina Felli, Davide Filardi, Riccardo Sergi, Luisa Maria Migneco, Massimo Giuseppe De Cesaris, Lorenzo Antonelli, Iolanda Francolini, Alessandra Gentili
{"title":"Exploring the extraction capabilities of natural cyclodextrin-nanosponges: The improvement moving from α- to γ-cyclodextrin-based polymers","authors":"Nina Felli, Davide Filardi, Riccardo Sergi, Luisa Maria Migneco, Massimo Giuseppe De Cesaris, Lorenzo Antonelli, Iolanda Francolini, Alessandra Gentili","doi":"10.1016/j.sampre.2025.100169","DOIUrl":"10.1016/j.sampre.2025.100169","url":null,"abstract":"<div><div>Cyclodextrins (CD) are cyclic oligosaccharides known for their capability to form inclusion complexes with molecules of appropriate size. CDs can also be used as polyfunctional monomers in polymerization reactions to prepare specialised sorbents with characteristics of biodegradability. In this work, different CD-based polymers, known as “nanosponges” (CDNS), were obtained using natural CDs (α-, β-, and γ-CD) as monomers, citric acid as the cross-linker and sodium dihydrogen phosphate (NaH<sub>2</sub>PO<sub>4</sub>) as the catalyst. CD cross-linking was confirmed by the carbonyl band shift in IR spectroscopy and the more complex degradation pathway in CDNS compared to CDs in thermogravimetric analysis. Scanning electron microscopy evidenced a porous structure of CDNS. Their sorption properties were investigated in the dispersive-solid phase extraction of 42 model compounds (common organic contaminants including drugs, hormones, herbicides, and pesticides) from river water samples. Among all the polymers, γ-CDNS exhibited the highest efficiency, achieving recoveries averaged on all the analytes of 67% and 79% at the concentration of 0.5 and 5 µg/L, respectively. Relative standard deviations were always below 20%. Detection limits ranged from 0.001 to 0.462 µg/L, while quantitation limits from 0.004 to 1.428 µg/L. The synthesized material is easy to produce, and the developed procedure enables the analysis of 10 samples/h, opening the door to new applications in sample preparation. Finally, the application of different metrics proved the environmental compatibility of the entire analytical procedure (AGREE score=0.55, and ComplexMoGAPI score=64) and the good practicability of the extraction method proposed (BAGI score > 60).</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100169"},"PeriodicalIF":5.2,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143577968","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Photini Papaioakeim , Efstathios A. Elia , Agapios Agapiou
{"title":"Monitoring of 12 DBPs in drinking water using a microextraction TD-GC-MS method","authors":"Photini Papaioakeim , Efstathios A. Elia , Agapios Agapiou","doi":"10.1016/j.sampre.2025.100168","DOIUrl":"10.1016/j.sampre.2025.100168","url":null,"abstract":"<div><div>Disinfection of drinking water is essential for ensuring public health; however, it leads to the formation of various undesirable disinfection by-products (DBPs). To comply with the recent European Union (EU) drinking water directive legislation (EU 2020/2184), a headspace HiSorb thermal desorption-gas chromatography-mass spectrometry (HS-HiSorb-TD-GC-MS) method was developed and validated for the quantification of 12 DBPs in drinking water. The HS-HiSorb-TD-GC-MS method presented high sensitivity and selectivity, linearity (1–120 ppb), limit of detection (LOD) 0.33–3.33 ppb, and limit of quantification (LOQ) 1–10 ppb. The method's accuracy was verified at three different concentrations, showing good repeatability (intra-day) and reproducibility (inter-day), ranging from 1.3 to 10 % and 3.3–15 %, respectively. Additionally, the method's recovery rates, at 10 ppb and 50 ppb, were estimated between 80 and 120 %. Water sample stability was also examined at various temperatures (4°C, 25°C, -20°C). The HS-HiSorb-TD-GC-MS method was used to investigate the presence of DBPs in tap water samples, highlighting its applicability to drinking water monitoring. The development of a green analytical method based on a sorbent-based sample preparation technique, contributes to sustainable and green analytical chemistry.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100168"},"PeriodicalIF":5.2,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143592453","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Assessment of the greenness of molecularly imprinted polymers used in sample preparation","authors":"Mariusz Marć , A. Martín-Esteban","doi":"10.1016/j.sampre.2025.100167","DOIUrl":"10.1016/j.sampre.2025.100167","url":null,"abstract":"<div><div>It is now widely accepted that the incorporation of molecularly imprinted polymers (MIPs) into sample preparation techniques has enabled unprecedented selectivity performance of analytical methods for the determination of a wide range of analytes in biological, food and environmental samples. However, according to the Principles of Green Chemistry and the subsequent Principles of Green Sample Preparation, it is clear that MIPs are far from being considered green materials, both due to the common harmful reagents and the experimental conditions used for their synthesis. Accordingly, new greener routes for MIP synthesis have been proposed in recent years. However, although the titles of some of the published papers include terms such as 'green MIP' or 'sustainable MIP', such improved properties have only been assessed intuitively and it is therefore unclear whether such claimed green or sustainable MIPs are actually so. Therefore, in the present review, published papers using apparently green MIPs in sample preparation were evaluated using the recently developed metric tool AGREEMIP. Such a tool is based on the assessment of 12 criteria related to the greenness of the different reagents used, energy requirements and other aspects of MIP synthesis procedures. The final values of performed AGREEMIP assessment ranged from 0.28 to 0.80. The scores obtained after the AGREEMIP assessment clearly show that, although slight improvements have been achieved in terms of greenness, there is an abuse of the use of green-related terms and further development is needed. In this context, some guidelines for greening MIPs are provided.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100167"},"PeriodicalIF":5.2,"publicationDate":"2025-03-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143561856","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Greener Solvents in Extraction of Proteins and Peptides","authors":"Katarína Maráková","doi":"10.1016/j.sampre.2025.100165","DOIUrl":"10.1016/j.sampre.2025.100165","url":null,"abstract":"<div><div>The sample pretreatment still represents a fundamental aspect of any analytical workflow, and the implementation of sustainable and efficient extraction of proteins is essential to satisfy the increasing requirements for high-quality extraction of proteins from their natural sources. Proteins, with their unique structural and functional characteristics, are utilized in several industries such as pharmaceuticals, biomedicine, cosmetics, and food. Traditional methods for protein extraction depend predominantly on hazardous organic solvents, thereby presenting both environmental and health-related risks. Recent progress has been directed towards developing environmentally benign alternative extraction approaches. Ionic liquids and deep eutectic solvents have demonstrated in the recent decade great potential as green solvents for protein extraction, thanks to their tunable properties that can be customized to various extraction protocols; thus, they are characterized by high selectivity. At the same time, they usually cause minimal denaturation of proteins, which is essential for normal functioning of proteins. However, the industrial implementation of these solvents still encounters obstacles, such as the knowledge gaps about their solvating characteristics, complexity in their synthesis (especially for ionic liquids), and potential for their reusability. The present review paper deals with the recent advances in the extraction of proteins and peptides with ionic liquids and deep eutectic solvents, discusses the influence of solvent characteristics on the extraction process, describes various extraction methods, and presents prospective future directions in this field.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"13 ","pages":"Article 100165"},"PeriodicalIF":5.2,"publicationDate":"2025-02-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143527263","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Fotouh R. Mansour , Alaa Bedair , Marcello Locatelli
{"title":"Click Analytical Chemistry Index as a novel concept and framework, supported with open source software to assess analytical methods","authors":"Fotouh R. Mansour , Alaa Bedair , Marcello Locatelli","doi":"10.1016/j.sampre.2025.100164","DOIUrl":"10.1016/j.sampre.2025.100164","url":null,"abstract":"<div><div>Click analytical chemistry (CAC) is a novel approach inspired by the principles of click chemistry, emphasizing simplicity, efficiency, and reliability. While click chemistry revolutionized synthetic methods, CAC aims to enhance chemical analysis by providing a framework for method assessment from a different perspective, focusing on improving the practicality and applicability of analytical techniques. In this work, we present the Click Analytical Chemistry Index (CACI) as a practical and user-friendly tool that provides both a metric and software solution for evaluating analytical methods. The software is available as an open source at <span><span>bit.ly/CACI2025</span><svg><path></path></svg></span>. The CACI system allows for objective and unbiased comparisons between techniques, encouraging the development of methods that are easier to implement without sacrificing performance. By promoting simplicity and practicality in method design, CACI supports the development of analytical procedures that not only meet rigorous performance standards but also simplify the analytical process. This work explores the principles and methodology of CAC and presents case studies that demonstrate its practical applications in advancing chemical analysis towards more efficient method development and evaluation.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100164"},"PeriodicalIF":5.2,"publicationDate":"2025-02-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143549844","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Polydopamine-graphene oxide aerogel for in-tube solid-phase microextraction of polycyclic aromatic hydrocarbons","authors":"Ziyi Jiang, Yanan Bu, Juanjuan Feng, Min Sun","doi":"10.1016/j.sampre.2024.100144","DOIUrl":"10.1016/j.sampre.2024.100144","url":null,"abstract":"<div><div>Due to the wide distribution and potential carcinogenicity, teratogenicity and mutagenicity, polycyclic aromatic hydrocarbons (PAHs) have attracted much attention, requiring efficient and sensitive methods for detection. In order to improve the stability and extraction performance of graphene oxide aerogel, polydopamine was introduced to functionalize it. Polydopamine-hybridized graphene oxide aerogel was in-situ fabricated on the surface of titanium wire. The composite material was characterized by SEM and FT-IR. Three aerogel-coated wires were filled in a polyetheretherketone tube for in-tube solid-phase microextraction. Coupled with high performance liquid chromatography, the tube showed good extraction performance for several PAHs. Under the optimal conditions (sampling volume of 60 mL, sampling rate of 1.50 mL/min, sample pH of 7.3, 0.5 % (v/v) of methanol and 1.0 % (w/v) of NaCl in sample, desorption time of 1.0 min), an online analytical method was developed for determining trace PAHs from water samples, with low detection limits (0.01–0.05 μg/L), wide linear ranges (0.03–50 μg/L, 0.15–100 μg/L) with correlation coefficients (0.9953–0.9992) and satisfactory repeatability (RSDs, 0.22 %-4.42 % for intra-day, 1.42 %-5.18 % for inter-day). The method was applied to analyze some water samples including leaching solutions of coal ash and paper food box, some targets were found. The recoveries in these samples with different spiked levels (2.0 and 10.0 μg/L) were in the range of 81–117 %.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"13 ","pages":"Article 100144"},"PeriodicalIF":5.2,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143130332","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yuqi Cheng , Jia Li , Xiaochen Xiu , Xinghua Teng , Wen Zhang , Lei Ji , Leilei Wang
{"title":"Nitrogen-rich covalent organic polymers for efficient solid phase extraction of nonsteroidal anti-inflammatory drugs from water samples","authors":"Yuqi Cheng , Jia Li , Xiaochen Xiu , Xinghua Teng , Wen Zhang , Lei Ji , Leilei Wang","doi":"10.1016/j.sampre.2025.100148","DOIUrl":"10.1016/j.sampre.2025.100148","url":null,"abstract":"<div><div>Non-steroidal anti-inflammatory drugs (NSAIDs) have received increasing attention owing to their ubiquitous occurrence in environmental water systems and adverse effects. In order to monitor trace levels of NSAIDs from complex water samples, development of facile and efficient sample pretreatment is of great significance. Herein, a nitrogen-rich covalent organic polymer containing phenyl, triazine and amine groups was fabricated via solvent-free copolymerization. Then, utilizing nitrogen-rich covalent organic polymer as adsorbent for solid phase extraction cartridges, the pretreatment method was combined with high-performance liquid chromatography-diode array detection to quantify five representative NSAIDs (ketoprofen, carprofen, flurbiprofen, diclofenac and mefenamic acid) in environmental water samples. Under the optimal extraction conditions (adsorbent amount: 40 mg; NaCl concentration: 0%; pH 6; extraction time: 20min; eluent solvent: 4 mL of formic acid/acetonitrile (5%, v/v)), the proposed method provided low detection limits (0.06–0.2 μg L<sup>-1</sup>), wide linear ranges (0.2–100 μg L<sup>-1</sup>) with correlation coefficients (0.9991–0.9997) and acceptable precision (RSDs, 6.6–8.5% for intra-day, 7.2–9.5% for inter-day). The practical application of the method was confirmed through the successful determination of NSAIDs in tap water, surface water, and sewage. The recoveries in these samples at the four NSAIDs concentration levels ranged from 81.3% to 109.8%, with the RSDs lower than 7.8%.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"13 ","pages":"Article 100148"},"PeriodicalIF":5.2,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143130412","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}