Natalia A. Gomez , Anabela S. Lorenzetti , Damian A. Uriarte , Carolina Acebal , Juan M. Padró , Antonio Canals , Mariano Garrido , Claudia E. Domini
{"title":"Revaluing optical techniques in the light of vortex- and ultrasound-assisted microextraction","authors":"Natalia A. Gomez , Anabela S. Lorenzetti , Damian A. Uriarte , Carolina Acebal , Juan M. Padró , Antonio Canals , Mariano Garrido , Claudia E. Domini","doi":"10.1016/j.sampre.2025.100179","DOIUrl":"10.1016/j.sampre.2025.100179","url":null,"abstract":"<div><div>The main objective of this review is to provide an overview of the coupling between microextraction techniques (mainly based on the use of vortex and ultrasound) and different optical techniques in order to demonstrate that their combination can be a valid and accessible option for the determination of chemical species at trace or ultra-trace level. This revaluation of conventional optical techniques, including detection by digital imaging, is related to the concept of democratic analytical chemistry, and refers to the possibility of generating quality results even in laboratories with limited resources and little access to sophisticated instrumentation. In addition, the development of greener solvents and new adsorbent materials expand the capacity and versatility of the microextraction techniques, making them more effective and environmentally friendly options. In summary, the article aims to draw the attention of researchers to techniques that usually fall into disuse but, in combination with appropriate preconcentration procedures, can be attractive and economical choices for routine analysis of organic and inorganic species.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100179"},"PeriodicalIF":5.2,"publicationDate":"2025-03-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143643203","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":"On the greenness of recent microwave-assisted digestion methods: An evaluation with AGREEprep","authors":"Juan L. Benedé , Francisco Pena-Pereira","doi":"10.1016/j.sampre.2025.100177","DOIUrl":"10.1016/j.sampre.2025.100177","url":null,"abstract":"<div><div>Microwave-assisted digestion (MAD) is a widely used technique for the preparation of samples for elemental analysis. Significant advances toward more efficient and less hazardous MAD methods have been described in recent years, even though no systematic evaluation has been carried out in terms of green sample preparation. The present work evaluates the effectiveness and environmental impact of recent MAD methods through the lens of AGREEprep, a recognized metric tool that identifies the greenness attributes of sample preparation methods. The metric tool was employed for the assessment of 38 decomposition methods for food analysis, including MAD methods involving decreasing amounts of oxidizing agents, considering supplemental reagents and assistances, such as oxygen pressure, hydrogen peroxide, ultraviolet irradiation, and microwave-induced combustion. In addition, conventional decomposition methods and alternative approaches involving infrared heating have been considered in the assessment. The 38 methods received overall scores in a wide range of 0.14 to 0.52, being MAD methods without acid consumption and those involving combustion the greenest methods (scores from 0.40 to 0.52). By systematically evaluating key criteria, such as reagent usage, energy consumption, process safety, and waste generation, AGREEprep provides a comprehensive view of MAD methods that can contribute to further improvements toward more sustainable analytical practices.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100177"},"PeriodicalIF":5.2,"publicationDate":"2025-03-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143681937","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}
Alejandra Molina-Balmaceda, Valentina Rojas-Candia, Juan José Triviño, Daniel Arismendi, Pablo Richter
{"title":"Grapefruit peel activated carbon for multi-analyte microextraction in water analysis through rotating disk sorptive extraction","authors":"Alejandra Molina-Balmaceda, Valentina Rojas-Candia, Juan José Triviño, Daniel Arismendi, Pablo Richter","doi":"10.1016/j.sampre.2025.100176","DOIUrl":"10.1016/j.sampre.2025.100176","url":null,"abstract":"<div><div>In the realm of green analytical chemistry, there is growing interest in sorbent phases derived from natural materials like grapefruit peels as promising alternatives to commercial sorbent phases. Initially, the effectiveness of grapefruit peels in their natural state was compared to activated carbons treated with activating agents as a sorbent phase in rotating disk sorptive extraction (RDSE). The conditions for synthesizing activated carbon were optimized by adjusting the activating agent variables, proportions, and temperatures to obtain an efficient material for extracting ethylparaben (EP), propylparaben (PP), ibuprofen (Ibu), triclosan (TCS), bisphenol A (BPA), and 17-α-ethinylestradiol (EE2) using rotating disk sorption extraction technique from aqueous samples. The optimal conditions were determined to be activation with ZnCl<sub>2</sub> at a 1:1.2 ratio (material: activating reagent) and carbonization at 400 °C (AC400(Z1.2)). Characterization revealed a hydrophilic microporous material with a large surface area and aromatic structure, confirming its potential as a sorbent phase for aqueous sample preparation. The application of AC400(Z1.2) sorbent phase in RDSE in river water confirmed its effectiveness, revealing EP, PP, Ibu, TCS, and BPA in concentrations ranging from 0.18 to 2.8 µg <span>l</span><sup>-1</sup>, with EE2 concentration below the limit of detection. Reusability studies demonstrate that this material can be reused for the simultaneous extraction of analytes in at least two consecutive extractions without requiring additional treatment between extractions. This material proves to be an economical and bio-based alternative to commercial sorbent phases. Finally, its application in RDSE was evaluated using green analytical chemistry metrics (AGREEprep and BAGI), resulting in a methodology with a low environmental impact.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100176"},"PeriodicalIF":5.2,"publicationDate":"2025-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143681877","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}
Ana Y. Simão , Luana M. Rosendo , Pedro Dinis , Cláudia Margalho , Maristela Andraus , Mário Barroso , Eugenia Gallardo
{"title":"Microextraction by packed sorbent for the determination of selected synthetic cathinones and 2C-P in hair","authors":"Ana Y. Simão , Luana M. Rosendo , Pedro Dinis , Cláudia Margalho , Maristela Andraus , Mário Barroso , Eugenia Gallardo","doi":"10.1016/j.sampre.2025.100175","DOIUrl":"10.1016/j.sampre.2025.100175","url":null,"abstract":"<div><div>New psychoactive substances (NPS), including synthetic cathinones and phenethylamines, pose significant challenges due to their evolving chemical structures and health impacts. This study aimed to optimize and validate a methodology for detecting and quantifying a number of synthetic cathinones [methylone, ethylone, pentedrone, 4-chloroethcathinone (4-CEC), penthylone, α-pyrrolidinopentiophenone (α-PVP), 3,4-methylenedioxypyrovalerone (MDPV), 4‑chloro-α-pyrrolidinovalerophenone (4-Cl-α-PVP), as well as phenethylamine 2,5-dimethoxy-4(n)-propylphenethylamine (2C-P)], in hair samples using microextraction by packed sorbent (MEPS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). We developed an environmentally friendly and cost-effective MEPS procedure, which was validated for selectivity, linearity, precision, accuracy, and recovery. Results demonstrated that the method effectively detects analytes with limits of quantification as low as 10 pg/mg. The method successfully identifies MDPV in concentrations consistent with those observed in chronic and acute drug consumption cases, proving its suitability in forensic and clinical toxicology. This approach offers a robust solution for forensic and clinical applications, by combining efficient sample clean-up with precise analytical capabilities.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100175"},"PeriodicalIF":5.2,"publicationDate":"2025-03-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143643202","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":"Spherical C18-functionalized ordered mesoporous silica packed on micro-solid phase extraction cartridges for simultaneous determination of twenty-three alkaloids in flower extract supplements","authors":"Begoña Fernández-Pintor , Judith Gañán , Damián Pérez-Quintanilla , Sonia Morante-Zarcero , Isabel Sierra","doi":"10.1016/j.sampre.2025.100174","DOIUrl":"10.1016/j.sampre.2025.100174","url":null,"abstract":"<div><div>A spherical ordered mesoporous silica functionalized with octadecylsilane ligand (SM-C18) was successfully synthesized and characterized, showing 647 m<sup>2</sup>/g of surface area, 45 Å of pore size, 4–6 μm of particle diameter and 0.37 mmol/g of functionalization degree. 1.5 mg of SM-C18 were packed into EPREP micro-solid phase extraction (µSPEed) cartridges for use with a handheld programmable digital analytical syringe (digiVOL®) to develop a sample preparation protocol for the analysis of two tropane (TAs) and twenty-one pyrrolizidine (PAs) alkaloids. The SM-C18 demonstrated greater retention capacity compared with commercial C18/hydrophilic amorphous silica sorbent. The optimized extraction conditions were as follows: 100 µL of methanol (2 cycles) and 100 µL of H<sub>2</sub>O (2 cycles) for conditioning, 100 µL of H<sub>2</sub>O-reconstituted sample (10 cycles), for a total of 1 mL of sample loaded, and 100 µL of methanol (2 cycles) for elution, followed by subsequent analysis by UHPLC-MS/MS. The method was successfully validated, showing good recoveries ranging between 91 and 97 %, low quantification limits and absence of matrix effect for the twenty-tree alkaloids. Additionally, cartridges packed with SM-C18 material allow for better reusability compared to the commercial material, as it has been demonstrated that they can be used for at least 75 extractions. This significantly enhances the method's sustainability. Finally, it was applied to 25 samples of flower extract supplements (FES). In two different batches of the sample obtained from <em>Convolvulus arvensis</em> flowers (FES4a and FES4b), atropine and scopolamine were quantified.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100174"},"PeriodicalIF":5.2,"publicationDate":"2025-03-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143629120","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}
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}