Advances in Sample Preparation最新文献

{"title":"Improved sample preparation using bead mill homogenization","authors":"Madison E. Walbrun ,&nbsp;Aamna Aijaz ,&nbsp;Gabriella Ryan ,&nbsp;John D. Bunting ,&nbsp;Zachary P. Morehouse ,&nbsp;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}

{"title":"Green solvents and enzymes combined with advanced extraction techniques for the recovery of bioactive carotenoids and extractable/non-extractable polyphenols from grapefruit peels","authors":"Gloria Domínguez-Rodríguez ,&nbsp;María Concepción García ,&nbsp;María Luisa Marina","doi":"10.1016/j.sampre.2025.100192","DOIUrl":"10.1016/j.sampre.2025.100192","url":null,"abstract":"<div><div>The simultaneous extraction of extractable phenolic compounds (EPPs) and carotenoids from grapefruit peels using microwave-assisted extraction (MAE) with biobased solvents was optimized, followed by non-extractable polyphenols (NEPs) extraction. Ethyl acetate:γ-valerolactone (20:80 v/v) yielded the highest antioxidant and anti-inflammatory EPPs at 50 °C in 6 min. From the residue, NEPs were obtained by comparing several methods: ultrasound-assisted extraction (UAE) combined with enzymatic-assisted extraction (EAE), and UAE and MAE with natural deep eutectic solvents (NaDES). UAE (15 min, 30 % amplitude) followed by EAE (70 °C, 40 min) and MAE-NaDES using choline chloride:lactic acid (1:2, 50 % water, 50 °C, 6 min) yielded the most bioactive NEPs. HPLC-DAD-QTOF-MS analysis allowed to identified 19 polyphenols in both extracts, highlighting naringin as the majority, particularly in UAE-EAE extract. Stability tests showed UAE-EAE extracts protect against oxidative damage, potentially extending the shelf life of food products. On the other hand, MAE-NaDES extracts prevent anti-inflammatory compound degradation, indicating their potential application in pharmaceutical formulations. Thus, depending on the purpose, either UAE-EAE or MAE-NaDES can be used.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100192"},"PeriodicalIF":5.2,"publicationDate":"2025-06-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144240816","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":"Innovative sample preparation techniques in food analysis: the rise of compressed fluids and novel solvents","authors":"Luana C. dos Santos ,&nbsp;Juan Felipe Grisales-Mejía ,&nbsp;Monique Martins Strieder ,&nbsp;Jose A. Mendiola ,&nbsp;Elena Ibáñez","doi":"10.1016/j.sampre.2025.100191","DOIUrl":"10.1016/j.sampre.2025.100191","url":null,"abstract":"<div><div>Compressed fluids and novel green solvents represent the most promising approaches for achieving sustainable sample preparation in food analysis. Traditional extraction techniques often rely on toxic organic solvents and energy-intensive processes, leading to environmental concerns and inefficient workflows. Green Analytical Chemistry (GAC) promotes the adoption of eco-friendly alternatives that minimize solvent consumption, reduce waste, and enhance extraction efficiency. This review explores the role of compressed fluids’ technologies, including Pressurized Liquid Extraction (PLE), Supercritical Fluid Extraction (SFE), and Gas-Expanded Liquid Extraction (GXL) as viable replacements for conventional solvent-based methods. These techniques offer high selectivity, shorter extraction times, and lower environmental impact. Additionally, novel solvents such as deep eutectic solvents (DES), bio-based alternatives, and gas-expanded liquids present sustainable solutions that improve biodegradability, safety, and solvent recyclability. By integrating these innovative approaches into analytical workflows, food analysis can align with Green Chemistry principles while maintaining high analytical performance. This review critically evaluates the latest advancements in green sample preparation techniques based on pressurized fluids, highlighting their transformative potential in food safety, authenticity verification, and bioactive compound extraction.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100191"},"PeriodicalIF":5.2,"publicationDate":"2025-05-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144168993","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":"Development of smart samplers and their comparison to dried serum spots for the analysis of growth hormone releasing hormone analogs using LCHRMS/MS","authors":"Christina Johannsen ,&nbsp;Anna Kha Tu Nguyen ,&nbsp;Sasha Shabani ,&nbsp;Inger Oulie ,&nbsp;Siri Dørum ,&nbsp;Yvette Dehnes ,&nbsp;Leon Reubsaet ,&nbsp;Trine Grønhaug Halvorsen","doi":"10.1016/j.sampre.2025.100190","DOIUrl":"10.1016/j.sampre.2025.100190","url":null,"abstract":"<div><div>Growth hormone-releasing hormone (GHRH) analogs, including sermorelin, CJC-1295, and tesamorelin, are prohibited in sports due to their performance-enhancing potential. Detecting these peptides remains challenging, requiring sensitive analytical techniques. This study explores the feasibility of dried serum spots (DSS) and smart samplers for detecting GHRH analogs in human serum using liquid chromatography-high-resolution tandem mass spectrometry. Smart samplers combine sampling and sample preparation in one tool; in this study smart samplers were developed using divinyl sulfone functionalized paper to immobilize antibodies for selective analyte capture. DSS and smart samplers were compared for extraction efficiency, precision, and detection capabilities. Various extraction approaches were evaluated to optimize analyte recovery followed by a blind sample study to assess detection capability at unknown concentrations. Results showed that DSS yielded higher overall signal intensities but exhibited greater variability. In contrast, smart samplers demonstrated improved reproducibility and sensitivity at lower concentrations. Smart samplers successfully identified sermorelin at 0.25 ng∙mL^-1, CJC-1295 at 4 ng∙mL^-1, and tesamorelin at 2.5 ng∙mL^-1, while DSS exhibited limitations at these concentrations. This study presents a proof-of-concept for using smart samplers and DSS in anti-doping analysis. While the results shown are promising, further optimization is needed to improve analyte recovery and sampler stability. The findings support the potential of alternative blood sampling techniques in doping control and peptide biomarker analysis.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100190"},"PeriodicalIF":5.2,"publicationDate":"2025-05-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144185228","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":"(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":"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":"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":"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":"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":"Natural deep eutectic solvent-based matrix solid-phase dispersion-ultrasound assisted extraction of pesticides in pears and their determination by liquid chromatography-tandem mass spectrometry","authors":"Ana Isabel García-Valcárcel,&nbsp;Esther Miguel,&nbsp;Antonio Martín-Esteban","doi":"10.1016/j.sampre.2025.100185","DOIUrl":"10.1016/j.sampre.2025.100185","url":null,"abstract":"<div><div>In recent years, natural deep eutectic solvents (NADES) have been proposed as sustainable solvents capable of replacing the conventional harmful organic solvents typically used in sample preparation. In this regard, in this work, several NADES have been evaluated for the development of a matrix solid phase dispersion - ultrasound-assisted extraction (MSPD-UAE) method for selected pesticides (thiamethoxam, thiacloprid, pirimicarb, acetamiprid and tebuconazole) from pear (peel and pulp) samples and final determination by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Among the different NADES and dispersants tested, the one consisting of choline chloride:1,3-propanediol in a 1:4 molar ratio combined with alumina showed the best performance. The effect of the amount of dispersant, the volume of NADES, the temperature of the ultrasonic bath and the duration of sonication was then optimised using response surface methodology (RSM) based on a four-factor, three-level Box-Behnken design. Under optimal conditions, no matrix effect was observed and quantitative recoveries, ranging from 78.5 to 120 % with relative standard deviations (RSDs) lower than 20 % were obtained, reaching limits of quantification within the range 4–10 ng g^-1, depending upon the analyte. In addition, after evaluation by Analytical Greenness Metric for Sample Preparation (AGREEprep), Sample Preparation Metric of Sustainability (SPMS) and Blue Applicability Grade Index (BAGI) metrics tools, the proposed method was found to be superior to other published methods in terms of safety and environmental impact with good applicability potential.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"14 ","pages":"Article 100185"},"PeriodicalIF":5.2,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143891022","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}