Advances in Sample Preparation最新文献_第5页

Innovative sample preparation techniques in food analysis: the rise of compressed fluids and novel solvents 食品分析中的创新样品制备技术：压缩流体和新型溶剂的兴起

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-05-23 DOI: 10.1016/j.sampre.2025.100191

Luana C. dos Santos , Juan Felipe Grisales-Mejía , Monique Martins Strieder , Jose A. Mendiola , Elena Ibáñez

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.

压缩流体和新型绿色溶剂代表了在食品分析中实现可持续样品制备的最有前途的方法。传统的提取技术通常依赖于有毒的有机溶剂和能源密集型工艺，导致环境问题和低效的工作流程。绿色分析化学（GAC）提倡采用环保的替代品，最大限度地减少溶剂消耗，减少浪费，提高提取效率。本文综述了压缩流体技术的作用，包括加压液体萃取（PLE）、超临界流体萃取（SFE）和气体膨胀液体萃取（GXL）作为传统溶剂基方法的可行替代品。这些技术具有高选择性、较短的提取时间和较低的环境影响。此外，新型溶剂，如深共晶溶剂（DES）、生物基替代品和气体膨胀液体，提供了可持续的解决方案，提高了生物降解性、安全性和溶剂可回收性。通过将这些创新的方法集成到分析工作流程中，食品分析可以与绿色化学原则保持一致，同时保持高分析性能。这篇综述批判性地评估了基于加压流体的绿色样品制备技术的最新进展，强调了它们在食品安全、真实性验证和生物活性化合物提取方面的变革潜力。

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引用次数: 0

Development of smart samplers and their comparison to dried serum spots for the analysis of growth hormone releasing hormone analogs using LCHRMS/MS LCHRMS/MS分析生长激素释放激素类似物的智能采样器的研制及其与干血清点的比较

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-05-22 DOI: 10.1016/j.sampre.2025.100190

Christina Johannsen , Anna Kha Tu Nguyen , Sasha Shabani , Inger Oulie , Siri Dørum , Yvette Dehnes , Leon Reubsaet , Trine Grønhaug Halvorsen

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.

生长激素释放激素（GHRH）类似物，包括血清素、CJC-1295和替沙莫瑞林，由于它们具有提高成绩的潜力，被禁止在体育运动中使用。检测这些肽仍然具有挑战性，需要灵敏的分析技术。本研究探讨了使用液相色谱-高分辨率串联质谱法检测人血清中GHRH类似物的干燥血清斑点（DSS）和智能采样器的可行性。智能采样器将采样和样品制备结合在一个工具中；在本研究中，使用二乙烯基砜功能化纸开发了智能采样器，用于固定抗体以进行选择性分析物捕获。比较了DSS和智能采样器的提取效率、精度和检测能力。评估了各种提取方法，以优化分析物回收率，随后进行了盲样研究，以评估未知浓度下的检测能力。结果表明，DSS产生了更高的整体信号强度，但表现出更大的变异性。相比之下，智能采样器在较低浓度下表现出更好的再现性和灵敏度。智能采样器成功地鉴定出0.25 ng∙mL-1的血清素、4 ng∙mL-1的CJC-1295和2.5 ng∙mL-1的替沙莫瑞林，而DSS在这些浓度下表现出局限性。本研究提出了在反兴奋剂分析中使用智能采样器和DSS的概念验证。虽然结果显示很有希望，但需要进一步优化以提高分析物回收率和进样器的稳定性。这些发现支持了替代血液采样技术在兴奋剂控制和肽生物标志物分析中的潜力。

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引用次数: 0

(Natural) deep eutectic solvents in food safety: Innovations in sample preparation 食品安全中的（天然）深共晶溶剂：样品制备的创新

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-05-01 DOI: 10.1016/j.sampre.2025.100188

Laura Carbonell-Rozas, Raquel Capilla-Flores, Roberto Romero-González, Antonia Garrido Frenich

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.

深共晶溶剂（DES）和天然深共晶溶剂（NADES）已成为传统有机溶剂的可持续和高效的替代品，用于食品安全分析。这些绿色溶剂符合绿色分析化学（GAC）的原则，为不同的分析应用提供可生物降解性、低毒性和高可调性。本文综述了（NA）DES在检测食品基质中污染物的样品制备中的作用，重点介绍了它们在提取农药、真菌毒素、药物、塑料添加剂、食品添加剂和重金属方面的有效性。它涵盖了多种样品制备技术和食品基质，涵盖了从2020年到现在发表的文献。详细讨论了（NA）DES的组成及其为特定食品安全应用量身定制的能力。它们与先进的萃取技术相结合，如分散液液微萃取（DLLME）、固相微萃取（SPME）和超声辅助萃取（UAE）。此外，探索了磁性和三元DES的潜力，以及其他新型DES变体。虽然一些共晶混合物的高粘度仍然是一个挑战，但创新的样品处理策略成功地缓解了这些限制，提高了在各种复杂食品基质中的提取效率和预富集能力。

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引用次数: 0

Novel gas-diffusion microextraction followed by gas chromatography coupled to tandem mass spectrometry methodology for the determination of fragrance allergens in cosmetic products 新型气相扩散微萃取-气相色谱-串联质谱法测定化妆品中香氛过敏原

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-05-01 DOI: 10.1016/j.sampre.2025.100187

Ana Castiñeira-Landeira , Angel Gomez-Feas , Antonia M. Carro , Thierry Dagnac , Paulo J. Almeida , Maria Llompart

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.

首次建立了气相扩散微萃取(GDME) -气相色谱-串联质谱（GC-MS/MS）联用的高效样品制备方法，用于测定水基和醇基化妆品中的香氛过敏原。从提取温度作为初步实验入手，优化了最显著的GDME参数。随后，进行了实验设计，以评估六个参数的影响：受体溶液体积、受体溶液中乙腈的百分比、样品稀释度、盐析效果、提取时间和样品体积。在优化条件下，对该方法进行了线性度、精密度、准确度等方面的验证，取得了较好的效果。经验证的方法应用于12个真实化妆品样品，表明这些过敏原在化妆品中广泛存在。值得注意的是，在一种化妆品中检测到460 μg mL-1的丁香，这是欧盟法规1223/2009禁止的化合物；部分样品中目标香氛过敏原的浓度达到1000 μg mL-1以上。该方法代表了一种可持续和实用的方法，分别得到AGREEPrep和BAGI指标的支持。

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引用次数: 0

Mass spectrometry-based high-throughput sample treatment methods for analysis of xenobiotics in human biofluids 基于质谱的高通量样品处理方法用于分析人体生物体液中的异种生物

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-05-01 DOI: 10.1016/j.sampre.2025.100183

Esther González-Infante , Anne San Román , Juan F. Ayala-Cabrera , Nestor Etxebarria , Belén González-Gaya , Naroa Lopez-Herguedas , Mikel Musatadi , Maitane Olivares , Ailette Prieto , Olatz Zuloaga

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.

本文综述了人体生物体液中有机异种生物质谱分析的高通量样品处理的最新进展。第一部分探讨了使用固体、液体和聚合物吸附剂的新兴技术，强调了增强批量处理和环境可持续性的配置。讨论了固相（微）萃取和液-液（微）萃取的新进展，以及吸附材料的新进展。此外，离心辅助样品处理被强调为一种补充技术，简化了关键步骤，包括蛋白质沉淀。还特别注意直接输注和基于环境电离的质谱法，它们通过消除色谱分离显着减少了分析时间。在临床和生物监测研究中，自动化对于处理大量样本至关重要。第二部分回顾了通过质谱法检测人体生物体液中有机外源物的高通量技术的最新应用。虽然主要重点是尿液和血液/血浆/血清，但也考虑到其他生物液体，如母乳、口服液、精液和脑脊液。大多数研究旨在通过自动化、批量处理或直接分析来提高样品吞吐量，而小型化和新型吸附剂的探索仍然较少。研究仍然主要集中在合法和非法的药物分析上，很少有研究涉及外源性的外来生物，如杀虫剂、工业化学品或干扰内分泌的化学物质。需要进一步努力开发能够在单一工作流程中检测广谱化合物的方法。最后，建立标准化的指标来定量评估超越传统优点的吞吐量，对于以有意义和普遍接受的方式定义高通量样品制备至关重要。

{"title":"Mass spectrometry-based high-throughput sample treatment methods for analysis of xenobiotics in human biofluids","authors":"Esther González-Infante , Anne San Román , Juan F. Ayala-Cabrera , Nestor Etxebarria , Belén González-Gaya , Naroa Lopez-Herguedas , Mikel Musatadi , Maitane Olivares , Ailette Prieto , 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}

引用次数: 0

Polymer inclusion membrane (PIM) extraction technique for assessing metal interactions with organic pollutants and microplastics in aquatic systems 聚合物包合膜（PIM）萃取技术评估水生系统中金属与有机污染物和微塑料的相互作用

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-05-01 DOI: 10.1016/j.sampre.2025.100184

Nasim Khatir, Berta Alcalde, Enriqueta Anticó, Clàudia Fontàs

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) > Zn(II) > 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.

本研究提出了一种研究水生环境中金属与污染物相互作用的新方法，基于聚合物包合膜（PIM）作为提取技术，用于提取二价金属离子(Ni（II), Cu（II）和Zn(II)）。pim被设计用于选择性地提取金属离子，为评估金属的游离部分提供了一种简单的方法，这对于了解其生物利用度和潜在毒性至关重要。PIM由40%的三乙酸纤维素（CTA）、30%的二（2-乙基己基）磷酸（D2EHPA）和30%的磷酸三丁酯（TBP）组成，能有效地促进Ni（II）、Cu（II）和Zn（II）进入0.5 M HNO3的接收相，其亲和力遵循Cu(II) >的趋势；锌(II)在镍(II)。在研究范围内（0.02 ~ 0.08 mM），所有金属与进料相的金属浓度和接收相的金属积累量呈线性趋势。此外，本研究首次探讨了这些金属与两种磺胺类抗生素，磺胺甲恶唑（SMX）和磺胺乙嗪（SMZ），以及两种微塑料：商业PVC和废塑料混合物的潜在相互作用。虽然推断在较高浓度下Cu（II）、Zn（II）和磺胺甲恶唑之间存在潜在的相互作用，但未观察到Ni（II）之间存在显著的相互作用。相反，在研究条件下，磺胺甲基嗪不表现出与任何金属离子的可测量的相互作用。此外，微塑料与金属的相互作用很弱或可以忽略不计，这表明在实验条件下对金属提取的影响很小。最后，应用pim萃取技术测量了受废弃矿山排水影响的河流水样中的游离锌水平，以及在与环境相关浓度的微塑料和SMX富集的同一基质中。

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引用次数: 0

The complex world of eutectic solvents: Guidelines for a correct characterization and use in sample preparation 共晶溶剂的复杂世界：在样品制备中正确表征和使用的指南

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-05-01 DOI: 10.1016/j.sampre.2025.100189

Chiara Dal Bosco, Massimo Giuseppe De Cesaris, Lorenzo Antonelli, Nina Felli, Alessandra Gentili

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.

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.

具有低温相变的混合物早在19世纪末就已为人所知，当时首次引入了“优生态”一词。一个重要的转折点出现在2003年，当时雅培和他的同事们创造了“深共晶溶剂”（DES）这个术语，用来描述熔点明显低于其单个组分的混合物。从那时起，这些系统吸引了越来越多的兴趣，并被广泛应用于化学的各个领域。然而，由于多年来缺乏严格和明确的定义，术语DES经常被误用。这导致了DESs（非理想体系）、共晶溶剂（ESs，热力学理想体系）和低转变温度混合物（LTTMs，亚稳体系）之间的混淆。这种歧义在分析化学中尤其明显，在分析化学中，术语DES经常被用作不完全表征的混合物的包罗万象的标签。在许多研究中，实际应用已经优先于彻底了解这些溶剂的物理化学性质。因此，通常缺乏基本的热力学数据，这妨碍了合理设计新系统和为特定目的选择最佳溶剂，特别是在萃取过程中。本文旨在通过具有代表性的例子和实际应用，阐明ESs、DESs和lttm的术语和分类。它追溯了这些独特溶剂的历史发展，并突出了它们在样品制备中的优势，局限性和多功能性。特别强调了水在调整提取效率方面的作用，以及使用计算工具来设计特定任务的DESs。提出了有用的指导方针，以正确的表征导致精确的分类和有效的应用。

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引用次数: 0

Towards a greener future: The role of sustainable methodologies in metabolomics research 迈向更绿色的未来：可持续方法在代谢组学研究中的作用

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-05-01 DOI: 10.1016/j.sampre.2025.100186

Chiara Spaggiari , Kgalaletso Othibeng , Fidele Tugizimana , Gabriele Rocchetti , Laura Righetti

Sustainability is a growing priority in scientific research, and metabolomics is no exception. Traditional metabolomics workflows rely on hazardous solvents, raising concerns regarding their environmental impact. Recent advancements in green analytical chemistry lay the ground for the integration of eco-friendly approaches in metabolomics from matrix collections and pre-treatment, through sample preparation till data analysis. This review explores the current state of sustainable metabolomic workflows, with a particular focus on green sample preparation methods, solvent-free, low-solvent extraction techniques, and energy-efficient instrumental analysis. Computational advancements, including AI-driven models, machine learning-based semi-quantification, and predictive algorithms for solvent selection, further enhance sustainability by reducing resource consumption. The applicability of these approaches in metabolomic studies, particularly in plant and food research is explored. By integrating innovative green methodologies across all stages of metabolomic workflows, researchers can significantly reduce environmental footprints while maintaining analytical rigor.

可持续性在科学研究中越来越受到重视，代谢组学也不例外。传统的代谢组学工作流程依赖于有害溶剂，这引起了人们对其环境影响的担忧。绿色分析化学的最新进展为代谢组学从基质收集和预处理到样品制备到数据分析的生态友好方法的整合奠定了基础。这篇综述探讨了可持续代谢组学工作流程的现状，特别关注绿色样品制备方法、无溶剂、低溶剂提取技术和节能仪器分析。计算方面的进步，包括人工智能驱动的模型、基于机器学习的半量化和溶剂选择的预测算法，通过减少资源消耗，进一步提高了可持续性。探讨了这些方法在代谢组学研究中的适用性，特别是在植物和食物研究中。通过在代谢组学工作流程的所有阶段集成创新的绿色方法，研究人员可以在保持分析严谨性的同时显着减少环境足迹。

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引用次数: 0

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 天然深共晶溶剂基基质固相分散-超声辅助提取梨中农药及液相色谱-串联质谱法测定

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-05-01 DOI: 10.1016/j.sampre.2025.100185

Ana Isabel García-Valcárcel, Esther Miguel, Antonio Martín-Esteban

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.

近年来，天然深共晶溶剂（NADES）被认为是一种可持续溶剂，能够取代传统的有害有机溶剂，通常用于样品制备。在这方面，本研究对几种NADES进行了评价，以建立基质固相分散-超声辅助提取（MSPD-UAE）方法，用于从梨（果皮和果肉）样品中提取农药（噻虫嗪、噻虫啉、吡虫威、啶虫啉和戊唑唑），并通过液相色谱-串联质谱（LC-MS/MS）进行最终测定。在不同的NADES和分散剂中，氯化胆碱：1,3-丙二醇以1:4的摩尔比与氧化铝复合的NADES和分散剂表现出最好的性能。然后利用响应面法（RSM），基于四因素、三级Box-Behnken设计，优化分散剂用量、NADES体积、超声浴温度和超声持续时间的影响。在最佳条件下，未观察到基质效应，定量回收率为78.5% ~ 120%，相对标准偏差（rsd）小于20%，根据分析物的不同，定量限在4 ~ 10 ng g-1。此外，通过对样品制备分析绿色度指标（AGREEprep）、可持续性样品制备指标（SPMS）和蓝色适用性等级指数（BAGI）指标工具的评价，发现该方法在安全性和环境影响方面优于其他已发表的方法，具有良好的适用性潜力。

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引用次数: 0

Recent trends in microsampling and reduced-volume sample preparation procedures 微型取样和减容样品制备程序的最新趋势

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-04-11 DOI: 10.1016/j.sampre.2025.100182

Miryam Perrucci , Erika Maria Ricci , Marcello Locatelli , Imran Ali , Fotou R. Mansour , Abuzar Kabir , Halil I. Ulusoy

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.

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.

绿色化学（GC）、绿色分析化学（GAC）和绿色样品制备（GSP）的出现对样品制备技术的发展产生了重大影响。这些方法的中心原则是减少样本量，并在色谱分析之前将溶剂和试剂的消耗降至最低。虽然这些进步促进了可持续性和分析效率，但一个持续的挑战在于开发创新技术，坚持这些原则，而不影响分析性能——分析化学的基本目标。在这种情况下，微采样技术的最新进展正在获得越来越多的关注。固相微萃取（SPME）和体积吸收微采样（VAMS）等技术正在被探索作为获得干燥生物基质（如血液、尿液和唾液）的有前途的工具，为干燥血液斑点（DBS）等传统方法提供了潜在的改进。此外，本文还讨论了旨在减少制备方案中所用样品和试剂体积的最新方法。本综述的主要目的是探讨微采样的最新趋势，并随后研究这些方法如何与不断发展的绿色样品制备景观相一致。

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