Advances in Sample Preparation最新文献

{"title":"A practical tutorial for optimizing electromembrane extraction methods by response surface methodology","authors":"Samira Dowlatshah ,&nbsp;Anne Oldeide Hay ,&nbsp;Line Noreng ,&nbsp;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":"2025-05-01","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}

{"title":"(Natural) deep eutectic solvents in food safety: Innovations in sample preparation","authors":"Laura Carbonell-Rozas,&nbsp;Raquel Capilla-Flores,&nbsp;Roberto Romero-González,&nbsp;Antonia Garrido Frenich","doi":"10.1016/j.sampre.2025.100188","DOIUrl":"10.1016/j.sampre.2025.100188","url":null,"abstract":"<div><div>Deep eutectic solvents (DES) and natural deep eutectic solvents (NADES) have emerged as sustainable and efficient alternatives to conventional organic solvents in food safety analysis. These green solvents align with the principles of green analytical chemistry (GAC) by offering biodegradability, low toxicity, and high tunability for different analytical applications. This review critically explores the role of (NA)DES in sample preparation for detecting contaminants in food matrices, highlighting their effectiveness in extracting pesticides, mycotoxins, pharmaceuticals, plastic additives, food additives, and heavy metals. It encompasses diverse sample preparation techniques and food matrices, covering literature published from 2020 to the present. A detailed discussion is provided on the compositions of (NA)DES and their tailor-made capabilities for specific food safety applications. Their integration with advanced extraction techniques such as dispersive liquid-liquid microextraction (DLLME), solid-phase microextraction (SPME), and ultrasound-assisted extraction (UAE) is provided. Additionally, the potential of magnetic and ternary DES is explored, along with other novel DES variants. While the high viscosity of some eutectic mixtures remains a challenge, innovative sample treatment strategies successfully mitigate these limitations, enhancing extraction efficiency and preconcentration capabilities across a wide range of complex food matrices.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100188"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143942574","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":"Revaluing optical techniques in the light of vortex- and ultrasound-assisted microextraction","authors":"Natalia A. Gomez ,&nbsp;Anabela S. Lorenzetti ,&nbsp;Damian A. Uriarte ,&nbsp;Carolina Acebal ,&nbsp;Juan M. Padró ,&nbsp;Antonio Canals ,&nbsp;Mariano Garrido ,&nbsp;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":"2025-05-01","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":"Novel gas-diffusion microextraction followed by gas chromatography coupled to tandem mass spectrometry methodology for the determination of fragrance allergens in cosmetic products","authors":"Ana Castiñeira-Landeira ,&nbsp;Angel Gomez-Feas ,&nbsp;Antonia M. Carro ,&nbsp;Thierry Dagnac ,&nbsp;Paulo J. Almeida ,&nbsp;Maria Llompart","doi":"10.1016/j.sampre.2025.100187","DOIUrl":"10.1016/j.sampre.2025.100187","url":null,"abstract":"<div><div>An efficient sample preparation method using gas-diffusion microextraction (GDME) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) is proposed for the first time to determine fragrance allergens in both aqueous and alcohol-based cosmetic products. The most significant GDME parameters were optimized, starting with extraction temperature as a preliminary experiment. Subsequently, an experimental design was performed to evaluate the influence of six parameters: acceptor solution volume, acetonitrile percentage in the acceptor solution, sample dilution, salting-out effect, extraction time, and sample volume. Under the optimized conditions, the method was validated in terms of linearity, precision, trueness, obtaining a good performance. The validated methodology was applied to twelve real cosmetic samples, demonstrating the widespread occurrence of these allergens in cosmetics. Notably, lilial, a compound prohibited by Regulation EC No 1223/2009, was detected in one cosmetic product (460 μg mL^-1); and the concentrations of some of the target fragrance allergens in some samples reach values above 1000 μg mL^-1. This methodology represents a sustainable and practical approach, supported by AGREEPrep and BAGI metrics, respectively.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100187"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143947570","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":"Polymer inclusion membrane (PIM) extraction technique for assessing metal interactions with organic pollutants and microplastics in aquatic systems","authors":"Nasim Khatir,&nbsp;Berta Alcalde,&nbsp;Enriqueta Anticó,&nbsp;Clàudia Fontàs","doi":"10.1016/j.sampre.2025.100184","DOIUrl":"10.1016/j.sampre.2025.100184","url":null,"abstract":"<div><div>This study presents a novel approach for studying metal-contaminant interactions in aquatic environments, based on a polymer inclusion membrane (PIM) as extraction technique, for the divalent metal ions (Ni(II), Cu(II), and Zn(II)). PIMs are designed to selectively extract metal ions, offering a simple method for assessing the free fraction of metals, which is crucial for understanding their bioavailability and potential toxicity. The PIM, composed of 40 % triacetate cellulose (CTA), 30 % di-(2-ethylhexyl) phosphoric acid (D2EHPA), and 30 % tributyl phosphate (TBP), efficiently facilitates the transport of Ni(II), Cu(II), and Zn(II) into a receiving phase of 0.5 M HNO₃, with the affinity following the trend Cu(II) &gt; Zn(II) &gt; Ni(II). All metals exhibit a linear trend in relation to the concentration of metal in the feed phase and the amount accumulated in the receiving phase, within the studied range (0.02 to 0.08 mM). Moreover, this research explores, for the first time, the potential interactions of these metals with two sulfonamide antibiotics, sulfamethoxazole (SMX) and sulfamethazine (SMZ), and two types of microplastics: commercial PVC and a blend of waste plastics. Although a potential interaction is inferred between Cu(II), Zn(II), and sulfamethoxazole at higher concentrations, no significant interaction is observed for Ni(II). In contrast, sulfamethazine does not exhibit measurable interactions with any of the metal ions under the conditions studied. Additionally, microplastics show weak or negligible interactions with the metals, suggesting a minimal impact on metal extraction under the experimental conditions. Finally, the PIM-extraction technique was applied to measure free Zn levels in a river water sample impacted by drainage from an abandoned mine, and in the same matrix enriched with microplastics and SMX at environmentally relevant concentrations.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100184"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143902529","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":"Mass spectrometry-based high-throughput sample treatment methods for analysis of xenobiotics in human biofluids","authors":"Esther González-Infante ,&nbsp;Anne San Román ,&nbsp;Juan F. Ayala-Cabrera ,&nbsp;Nestor Etxebarria ,&nbsp;Belén González-Gaya ,&nbsp;Naroa Lopez-Herguedas ,&nbsp;Mikel Musatadi ,&nbsp;Maitane Olivares ,&nbsp;Ailette Prieto ,&nbsp;Olatz Zuloaga","doi":"10.1016/j.sampre.2025.100183","DOIUrl":"10.1016/j.sampre.2025.100183","url":null,"abstract":"<div><div>This review examines recent advancements in high-throughput sample treatment for mass spectrometric analysis of organic xenobiotics in human biofluids. The first section explores emerging techniques using solid, liquid and polymeric sorbents, emphasizing configurations that enhance batch processing and environmental sustainability. Innovations in solid-phase (micro)extraction and liquid-liquid (micro)extraction are discussed, along with advancements in sorbent materials. Additionally, centrifugal-assisted sample treatment is highlighted as a complementary technique that streamlines key steps, including protein precipitation. Special attention is also given to direct infusion and ambient ionization-based mass spectrometry, which significantly reduce analysis time by eliminating chromatographic separation. Automation, crucial for handling large sample volumes in clinical and biomonitoring studies, is also emphasized. The second section reviews recent applications of high-throughput techniques for detecting organic xenobiotics in human biofluids via mass spectrometry. While the primary focus is on urine and blood/plasma/serum, other biofluids such as breast milk, oral fluid, semen and cerebrospinal fluid are also considered. Most studies aim to increase sample throughput via automation, batch processing, or direct analysis, while miniaturization and novel sorbents remain less explored. Research remains largely centered on legal and illegal drug analysis, with fewer studies addressing exogenous xenobiotics such as pesticides, industrial chemicals, or endocrine-disrupting chemicals. Further efforts are needed to develop methods capable of detecting a broad spectrum of compounds within a single workflow. Finally, establishing standardized metrics to quantitatively assess throughput beyond traditional figures of merit is essential for defining high-throughput sample preparation in a meaningful and universally accepted manner.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100183"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143907504","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":"Exploring the extraction capabilities of natural cyclodextrin-nanosponges: The improvement moving from α- to γ-cyclodextrin-based polymers","authors":"Nina Felli,&nbsp;Davide Filardi,&nbsp;Riccardo Sergi,&nbsp;Luisa Maria Migneco,&nbsp;Massimo Giuseppe De Cesaris,&nbsp;Lorenzo Antonelli,&nbsp;Iolanda Francolini,&nbsp;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 (NaH₂PO₄) 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 &gt; 60).</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100169"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","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}

{"title":"The complex world of eutectic solvents: Guidelines for a correct characterization and use in sample preparation","authors":"Chiara Dal Bosco,&nbsp;Massimo Giuseppe De Cesaris,&nbsp;Lorenzo Antonelli,&nbsp;Nina Felli,&nbsp;Alessandra Gentili","doi":"10.1016/j.sampre.2025.100189","DOIUrl":"10.1016/j.sampre.2025.100189","url":null,"abstract":"<div><div>Mixtures with low-temperature phase transitions have been known since the late 19th century, when the term “eutaxia” was first introduced. A major turning point came in 2003, when Abbott and colleagues coined the term “deep eutectic solvent” (DES) to describe mixtures whose melting points are significantly lower than those of their individual components. Since then, these systems have attracted growing interest and have widely been applied across various areas of Chemistry. However, the term DES has often been misused due to the lack of a strict and clear definition for many years. This has led to confusion among DESs (non-ideal systems), eutectic solvents (ESs, thermodynamically ideal systems), and low transition temperature mixtures (LTTMs, metastable systems). This ambiguity is especially pronounced in Analytical Chemistry, where the term DES is frequently used as a catch-all label for not-well characterized mixtures. In many studies, practical applications have been prioritized over a thorough understanding of the physicochemical nature of these solvents. As a result, essential thermodynamic data are often lacking, which hinders the rational design of new systems and the selection of optimal solvents for specific purposes, particularly in extraction processes.</div><div>This review aims to clarify the terminology and classification of ESs, DESs, and LTTMs through representative examples and practical applications. It traces the historical development of these unique solvents and highlights their strengths, limitations, and versatility in sample preparation. Special emphasis is placed on the role of water in tuning extraction efficiency and on the use of computational tools to design task-specific DESs. Helpful guidelines are proposed for a proper characterization leading to an precise classification and effective application.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100189"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144107614","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":"Monitoring of 12 DBPs in drinking water using a microextraction TD-GC-MS method","authors":"Photini Papaioakeim ,&nbsp;Efstathios A. Elia ,&nbsp;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":"2025-05-01","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":"Recent trends in microsampling and reduced-volume sample preparation procedures","authors":"Miryam Perrucci ,&nbsp;Erika Maria Ricci ,&nbsp;Marcello Locatelli ,&nbsp;Imran Ali ,&nbsp;Fotou R. Mansour ,&nbsp;Abuzar Kabir ,&nbsp;Halil I. Ulusoy","doi":"10.1016/j.sampre.2025.100182","DOIUrl":"10.1016/j.sampre.2025.100182","url":null,"abstract":"<div><div>The emergence of Green Chemistry (GC), Green Analytical Chemistry (GAC), and Green Sample Preparation (GSP) has significantly influenced the evolution of sample preparation techniques. A central tenet of these approaches is the reduction of sample size, and the minimization of solvent and reagent consumption prior to chromatographic analysis. While these advancements promote sustainability and analytical efficiency, a persistent challenge lies in developing innovative techniques that adhere to these principles without compromising analytical performance-the fundamental goal of analytical chemistry.</div><div>In this context, recent advancements in microsampling techniques are gaining increased attention. Techniques such as Solid-Phase Microextraction (SPME) and Volumetric Absorptive Microsampling (VAMS) are being explored as promising tools for obtaining dried biological matrices, such as blood, urine, and saliva offering potential improvements over traditional methods like Dried Blood Spotting (DBS). Moreover, this review discusses recent methods designed to reduce the volume of samples and reagents used in preparation protocols. The primary aim of this review is to explore the latest trends in microsampling and, subsequently, to examine how these methods align with the evolving landscape of green sample preparation.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100182"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143829286","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}