Advances in Sample Preparation最新文献_第6页

On the greenness of recent microwave-assisted digestion methods: An evaluation with AGREEprep 最近几种微波辅助消化方法的绿度评价：用AGREEprep进行评价

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-03-16 DOI: 10.1016/j.sampre.2025.100177

Juan L. Benedé , Francisco Pena-Pereira

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.

微波辅助消解（MAD）是一种广泛应用于元素分析样品制备的技术。近年来，尽管在绿色样品制备方面没有进行系统的评估，但在更有效和更低危害的MAD方法方面取得了重大进展。目前的工作通过AGREEprep（一种识别样品制备方法的绿色属性的公认度量工具）的镜头来评估最近MAD方法的有效性和环境影响。该计量工具用于评估38种食品分析分解方法，包括减少氧化剂量的MAD方法，考虑补充试剂和辅助试剂，如氧压、过氧化氢、紫外线照射和微波诱导燃烧。此外，在评估中还考虑了传统的分解方法和涉及红外加热的替代方法。38种方法的总体得分在0.14到0.52之间，其中没有酸消耗的MAD方法和涉及燃烧的方法是最环保的方法（得分从0.40到0.52）。通过系统地评估关键标准，如试剂使用、能源消耗、过程安全性和废物产生，AGREEprep提供了MAD方法的全面视图，可以有助于进一步改进更可持续的分析实践。

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引用次数: 0

Grapefruit peel activated carbon for multi-analyte microextraction in water analysis through rotating disk sorptive extraction 葡萄柚皮活性炭用于多分析物微萃取水中分析，通过旋转圆盘吸附萃取

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-03-15 DOI: 10.1016/j.sampre.2025.100176

Alejandra Molina-Balmaceda, Valentina Rojas-Candia, Juan José Triviño, Daniel Arismendi, Pablo Richter

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 ZnCl₂ 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 l^-1, 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.

在绿色分析化学领域，人们对从葡萄柚皮等天然材料中提取的吸附剂相越来越感兴趣，认为这是商业吸附剂相的有前途的替代品。首先，在旋转圆盘吸附萃取（RDSE）中，将天然状态下的葡萄柚皮与活性炭作为吸附剂处理后的效果进行了比较。通过调整活化剂的变量、比例和温度，优化了活性炭的合成条件，得到了一种高效提取对羟基苯甲酸乙酯（EP）、对羟基苯甲酸丙酯（PP）、布洛芬（Ibu）、三氯生（TCS）、双酚A （BPA）和17-α-炔雌醇（EE2）的材料。结果表明，最佳活化条件为：ZnCl2以1:2 .2的比例（材料：活化剂）活化，400℃（AC400(Z1.2)）炭化。表征揭示了具有大表面积和芳香结构的亲水性微孔材料，证实了其作为水样品制备的吸附剂相的潜力。AC400（Z1.2）吸附剂相对河水中RDSE的吸附效果得到了验证，EP、PP、Ibu、TCS和BPA的浓度在0.18 ~ 2.8µg l-1之间，EE2的浓度低于检测限。可重复使用性研究表明，该材料可以在至少两次连续提取中重复使用，而不需要在提取之间进行额外的处理。这种材料被证明是一种经济和生物基的替代商业吸附剂相。最后，利用绿色分析化学指标（AGREEprep和BAGI）对其在RDSE中的应用进行了评估，得出了一种低环境影响的方法。

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引用次数: 0

Microextraction by packed sorbent for the determination of selected synthetic cathinones and 2C-P in hair 填充吸附剂微萃取法测定头发中合成卡西酮和2C-P的含量

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-03-14 DOI: 10.1016/j.sampre.2025.100175

Ana Y. Simão , Luana M. Rosendo , Pedro Dinis , Cláudia Margalho , Maristela Andraus , Mário Barroso , Eugenia Gallardo

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.

新型精神活性物质（NPS），包括合成卡西酮和苯乙胺，由于其化学结构不断演变和对健康的影响，构成了重大挑战。本研究旨在优化和验证一种检测和定量合成卡西酮[甲酮、乙炔、戊酮、4-氯卡西酮（4- cec）、戊酮、α-吡咯烷二酮（α-PVP）、3,4-亚甲基二氧基戊酮（MDPV）、4-氯-α-吡咯烷二酮（4- cl -α-PVP）和苯乙胺2,5-二甲氧基-4(n)-丙基苯乙胺（2C-P）]的方法。利用填充吸附剂（MEPS）微萃取和液相色谱-串联质谱（LC-MS/MS）对头发样品进行分析。我们开发了一种环境友好且经济高效的MEPS程序，并对其选择性、线性度、精密度、准确度和回收率进行了验证。结果表明，该方法可有效检测分析物，定量限低至10 pg/mg。该方法成功地鉴定出MDPV浓度与慢性和急性吸毒病例中观察到的浓度一致，证明了其在法医和临床毒理学上的适用性。这种方法结合了高效的样品清理和精确的分析能力，为法医和临床应用提供了强大的解决方案。

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引用次数: 0

Spherical C18-functionalized ordered mesoporous silica packed on micro-solid phase extraction cartridges for simultaneous determination of twenty-three alkaloids in flower extract supplements 球形c18功能化有序介孔二氧化硅填充微固相萃取筒，用于同时测定花提取物中23种生物碱

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-03-11 DOI: 10.1016/j.sampre.2025.100174

Begoña Fernández-Pintor , Judith Gañán , Damián Pérez-Quintanilla , Sonia Morante-Zarcero , Isabel Sierra

A spherical ordered mesoporous silica functionalized with octadecylsilane ligand (SM-C18) was successfully synthesized and characterized, showing 647 m²/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 H₂O (2 cycles) for conditioning, 100 µL of H₂O-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 Convolvulus arvensis flowers (FES4a and FES4b), atropine and scopolamine were quantified.

成功合成了十八烷基硅烷配体功能化的球形有序介孔二氧化硅（SM-C18），其比表面积为647 m2/g，孔径为45 Å，粒径为4 ~ 6 μm，功能化度为0.37 mmol/g。将1.5 mg SM-C18装进EPREP微固相萃取（µSPEed）盒中，与手持式可编程数字分析注射器（digiVOL®）一起使用，以制定样品制备方案，用于分析两种tropane （TAs）和21种pyrrolizidine （PAs）生物碱。与商用C18/亲水无定形二氧化硅吸附剂相比，SM-C18表现出更大的保留容量。优化的提取条件为：100µL甲醇（2个循环）和100µL H2O（2个循环），100µL水重构样品（10个循环），共装样1ml， 100µL甲醇（2个循环）洗脱，UHPLC-MS/MS分析。结果表明，该方法回收率在91% ~ 97%之间，定量限低，不存在基质效应。此外，与商业材料相比，SM-C18材料包装的墨盒具有更好的可重复使用性，因为已经证明它们可以用于至少75次提取。这大大提高了该方法的可持续性。最后，将其应用于25个花提取物补充剂（FES）样品。对两批旋花FES4a和FES4b样品中阿托品和东莨菪碱进行定量分析。

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引用次数: 0

Advances in microextraction techniques utilizing deep eutectic solvents for the extraction of antibiotics 利用深共晶溶剂萃取抗生素的微萃取技术进展

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-03-07 DOI: 10.1016/j.sampre.2025.100172

Mussab Uddin , Faizah Mohammad Yunus , Zaharaddeen Muhammad , Muggundha Raoov , Andrew William King , Waleed Alahmad , Sibel A. Ozkan

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.

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.

食品、水和环境基质中抗生素污染的出现要求开发高效、敏感和环境可持续的分析方法。深共晶溶剂（DESs）由于其可调的特性、低毒性和可生物降解性，作为传统溶剂的绿色替代品而受到广泛关注。本文综述了基于des的微萃取技术在抗生素检测中的最新进展，包括固相微萃取、液-液微萃取和涡流辅助方法。与高效液相色谱-质谱和离子迁移谱等尖端分析仪器的结合，提高了微量抗生素的选择性和敏感性。关键的挑战，如DES粘度和可扩展性，以及新兴的解决方案，包括新的DES配方和功能性添加剂，以提高萃取效率，进行了严格的审查。这篇综述强调了基于des的微萃取在促进绿色分析实践中的作用，并强调了其在环境监测、药物残留分析和食品安全方面的广泛应用潜力。通过确定当前的局限性并为未来的研究提供策略，本综述为推进可持续的抗生素提取方法提供了宝贵的资源。

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引用次数: 0

Recent advances in environmental sample preparation: Nanomaterials, automation, and sustainable strategies 环境样品制备的最新进展：纳米材料、自动化和可持续策略

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-03-05 DOI: 10.1016/j.sampre.2025.100171

Federico Belén , Julián Gutiérrez , Valeria Springer

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.

随着环境基质中微污染物的不断增加以及对其进行监测的需要，人们需要更有效和准确的分析方法。特别是，样品制备程序是必要的，以解决环境样品的复杂性，同时确保高灵敏度。为了满足这些需求，各种纳米材料（NMs）被提出作为萃取相来发展小型化吸附剂萃取方法。这些纳米材料，从碳基纳米结构和金属基或金属氧化物纳米颗粒，到金属有机复合材料，都处于创新的前沿，因为它们具有特殊的表面积，可调的性能，易于功能化，在某些情况下，绿色生产路线。另一方面，（半）自动化平台的发展促进了高通量和可重复的样品处理，显著减少了试剂、时间和劳动力的使用。这篇综述强调了NMs和自动化在过去五年中在推进样品制备方法方面的关键作用，与绿色样品制备（GSP）指南保持一致。此外，在开发现代样品制备方法的背景下，讨论了新兴技术（如3D打印）的集成。最近的贡献包括小型化平台、绿色纳米吸附剂和自动化处理步骤的集成，它们有潜力为监测环境基质中的微污染物提供高效、经济的解决方案。

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引用次数: 0

A practical tutorial for optimizing electromembrane extraction methods by response surface methodology 用响应面法优化电膜提取方法的实用教程

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-03-04 DOI: 10.1016/j.sampre.2025.100170

Samira Dowlatshah , Anne Oldeide Hay , Line Noreng , Frederik André Hansen

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.

微萃取技术，如电膜萃取（EME），通过提供高效、经济、环保的样品制备方法，极大地促进了分析化学的发展。EME对于可电离分析物尤其有前景，其成功依赖于优化多个实验变量。传统上，优化采用了一次一个变量（OVAT）的方法，这种方法既耗时又可能忽略变量之间的相互作用。本教程介绍了响应面方法（RSM），它是优化EME方法的一种较好的替代方法。RSM允许多种因素同时变化，用较少的实验提供对其影响和相互作用的全面理解。本教程涵盖了EME的基本原理、基本实验参数以及RSM在方法优化中的应用。它包括对软件选择、设计选择、因素设置、响应定义和多个响应的优化的指导。进行实验，分析数据和解释模型的实际步骤是详细的，用现实生活中的例子来说明这个过程。本教程的目的是使RSM的新手和中等经验的用户访问，促进其在分析化学更广泛的应用。通过简化复杂的优化过程，本教程支持开发健壮、高效和绿色的EME方法。

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引用次数: 0

Exploring the extraction capabilities of natural cyclodextrin-nanosponges: The improvement moving from α- to γ-cyclodextrin-based polymers 探索天然环糊精纳米海绵的提取能力：从α-到γ-环糊精聚合物的改进

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-03-03 DOI: 10.1016/j.sampre.2025.100169

Nina Felli, Davide Filardi, Riccardo Sergi, Luisa Maria Migneco, Massimo Giuseppe De Cesaris, Lorenzo Antonelli, Iolanda Francolini, Alessandra Gentili

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 > 60).

环糊精（CD）是一种环状低聚糖，以其与适当大小的分子形成包合物的能力而闻名。cd还可以作为多官能单体用于聚合反应，制备具有生物降解特性的专用吸附剂。在这项工作中，以天然cd （α-， β-和γ-CD）为单体，柠檬酸为交联剂，磷酸二氢钠（NaH2PO4）为催化剂，制备了不同的cd基聚合物，称为“纳米海绵”（CDNS）。红外光谱的羰基带移证实了CD的交联，热重分析证实了CDNS的降解途径比CD更复杂。扫描电镜显示CDNS具有多孔结构。研究了它们在分散固相萃取中对42种模型化合物（包括药物、激素、除草剂和杀虫剂等常见有机污染物）的吸附性能。其中，γ-CDNS效率最高，在0.5µg/L和5µg/L浓度下，平均回收率分别为67%和79%。相对标准偏差均在20%以下。检出限为0.001 ~ 0.462µg/L，定量限为0.004 ~ 1.428µg/L。合成材料易于生产，开发的程序可以分析10个样品/小时，为样品制备的新应用打开了大门。最后，不同指标的应用证明了整个分析过程的环境相容性（AGREE评分=0.55，ComplexMoGAPI评分=64）和所提出的提取方法的良好实用性(BAGI评分>；60）.

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引用次数: 0

Monitoring of 12 DBPs in drinking water using a microextraction TD-GC-MS method 微萃取TD-GC-MS法监测饮用水中12种DBPs

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-03-03 DOI: 10.1016/j.sampre.2025.100168

Photini Papaioakeim , Efstathios A. Elia , Agapios Agapiou

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.

饮用水消毒对确保公众健康至关重要；然而，它会导致各种不良消毒副产物（DBPs）的形成。为符合欧盟饮用水指令立法（EU 2020/2184），建立了顶空HiSorb热解吸-气相色谱-质谱（HS-HiSorb-TD-GC-MS）方法，并对其进行了验证，用于饮用水中12种DBPs的定量分析。HS-HiSorb-TD-GC-MS方法具有较高的灵敏度和选择性，线性度（1 ~ 120 ppb），检出限（LOD） 0.33 ~ 3.33 ppb，定量限（LOQ） 1 ~ 10 ppb。在3种不同浓度下验证了方法的准确性，重复性（日内）和再现性（日内）较好，范围分别为1.3 ~ 10%和3.3 ~ 15%。此外，该方法在10 ppb和50 ppb下的回收率估计在80%到120%之间。在不同温度（4°C, 25°C, -20°C）下也检测了水样的稳定性。采用HS-HiSorb-TD-GC-MS方法对自来水样品中DBPs的存在情况进行了调查，突出了其在饮用水监测中的适用性。基于吸附剂样品制备技术的绿色分析方法的发展，有助于可持续发展和绿色分析化学。

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引用次数: 0

Assessment of the greenness of molecularly imprinted polymers used in sample preparation 评估用于样品制备的分子印迹聚合物的绿色环保性

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-03-02 DOI: 10.1016/j.sampre.2025.100167

Mariusz Marć , A. Martín-Esteban

It is now widely accepted that the incorporation of molecularly imprinted polymers (MIPs) into sample preparation techniques has enabled unprecedented selectivity performance of analytical methods for the determination of a wide range of analytes in biological, food and environmental samples. However, according to the Principles of Green Chemistry and the subsequent Principles of Green Sample Preparation, it is clear that MIPs are far from being considered green materials, both due to the common harmful reagents and the experimental conditions used for their synthesis. Accordingly, new greener routes for MIP synthesis have been proposed in recent years. However, although the titles of some of the published papers include terms such as 'green MIP' or 'sustainable MIP', such improved properties have only been assessed intuitively and it is therefore unclear whether such claimed green or sustainable MIPs are actually so. Therefore, in the present review, published papers using apparently green MIPs in sample preparation were evaluated using the recently developed metric tool AGREEMIP. Such a tool is based on the assessment of 12 criteria related to the greenness of the different reagents used, energy requirements and other aspects of MIP synthesis procedures. The final values of performed AGREEMIP assessment ranged from 0.28 to 0.80. The scores obtained after the AGREEMIP assessment clearly show that, although slight improvements have been achieved in terms of greenness, there is an abuse of the use of green-related terms and further development is needed. In this context, some guidelines for greening MIPs are provided.

现在人们普遍认为，将分子印迹聚合物（MIPs）结合到样品制备技术中，可以使分析方法具有前所未有的选择性，用于测定生物、食品和环境样品中的各种分析物。然而，根据绿色化学原理和随后的绿色样品制备原理，很明显，由于常见的有害试剂和用于合成它们的实验条件，MIPs远未被认为是绿色材料。因此，近年来提出了新的更环保的MIP合成路线。然而，尽管一些已发表的论文的标题包括“绿色MIP”或“可持续MIP”等术语，但这种改进的性能只是直观地进行了评估，因此尚不清楚这些声称的绿色或可持续MIP是否真的如此。因此，在本综述中，在样品制备中使用明显绿色MIPs的已发表论文使用最近开发的度量工具AGREEMIP进行评估。该工具基于对12个标准的评估，这些标准与所使用的不同试剂的绿色度、能量要求和MIP合成过程的其他方面有关。执行的AGREEMIP评估的最终值范围为0.28至0.80。AGREEMIP评估后获得的分数清楚地表明，虽然在绿色方面取得了轻微的进步，但绿色相关术语的使用存在滥用，需要进一步发展。在此背景下，提供了一些绿化MIPs的准则。

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