Advances in Sample Preparation最新文献_第7页

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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引用次数: 0

Greener Solvents in Extraction of Proteins and Peptides 绿色溶剂在蛋白质和多肽提取中的应用

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-25 DOI: 10.1016/j.sampre.2025.100165

Katarína Maráková

The sample pretreatment still represents a fundamental aspect of any analytical workflow, and the implementation of sustainable and efficient extraction of proteins is essential to satisfy the increasing requirements for high-quality extraction of proteins from their natural sources. Proteins, with their unique structural and functional characteristics, are utilized in several industries such as pharmaceuticals, biomedicine, cosmetics, and food. Traditional methods for protein extraction depend predominantly on hazardous organic solvents, thereby presenting both environmental and health-related risks. Recent progress has been directed towards developing environmentally benign alternative extraction approaches. Ionic liquids and deep eutectic solvents have demonstrated in the recent decade great potential as green solvents for protein extraction, thanks to their tunable properties that can be customized to various extraction protocols; thus, they are characterized by high selectivity. At the same time, they usually cause minimal denaturation of proteins, which is essential for normal functioning of proteins. However, the industrial implementation of these solvents still encounters obstacles, such as the knowledge gaps about their solvating characteristics, complexity in their synthesis (especially for ionic liquids), and potential for their reusability. The present review paper deals with the recent advances in the extraction of proteins and peptides with ionic liquids and deep eutectic solvents, discusses the influence of solvent characteristics on the extraction process, describes various extraction methods, and presents prospective future directions in this field.

样品预处理仍然是任何分析工作流程的一个基本方面，实现可持续和高效的蛋白质提取对于满足从天然来源提取高质量蛋白质的日益增长的要求至关重要。蛋白质以其独特的结构和功能特点，广泛应用于制药、生物医药、化妆品、食品等行业。传统的蛋白质提取方法主要依赖于有害的有机溶剂，因此存在环境和健康风险。最近的进展是针对开发对环境无害的替代提取方法。近十年来，离子液体和深共晶溶剂作为蛋白质提取的绿色溶剂表现出了巨大的潜力，这要归功于它们可调的特性，可以定制各种提取方案；因此，它们具有高选择性的特点。同时，它们通常会引起蛋白质的最小变性，这对蛋白质的正常功能是必不可少的。然而，这些溶剂的工业实施仍然遇到障碍，例如关于它们的溶剂化特性的知识差距，它们的合成复杂性（特别是离子液体），以及它们的可重用性的潜力。本文综述了离子液体和深度共晶溶剂提取蛋白质和多肽的最新进展，讨论了溶剂特性对提取过程的影响，介绍了各种提取方法，并展望了该领域的未来发展方向。

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引用次数: 0

Click Analytical Chemistry Index as a novel concept and framework, supported with open source software to assess analytical methods 点击分析化学指数作为一个新的概念和框架，与开源软件的支持，以评估分析方法

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-23 DOI: 10.1016/j.sampre.2025.100164

Fotouh R. Mansour , Alaa Bedair , Marcello Locatelli

Click analytical chemistry (CAC) is a novel approach inspired by the principles of click chemistry, emphasizing simplicity, efficiency, and reliability. While click chemistry revolutionized synthetic methods, CAC aims to enhance chemical analysis by providing a framework for method assessment from a different perspective, focusing on improving the practicality and applicability of analytical techniques. In this work, we present the Click Analytical Chemistry Index (CACI) as a practical and user-friendly tool that provides both a metric and software solution for evaluating analytical methods. The software is available as an open source at bit.ly/CACI2025. The CACI system allows for objective and unbiased comparisons between techniques, encouraging the development of methods that are easier to implement without sacrificing performance. By promoting simplicity and practicality in method design, CACI supports the development of analytical procedures that not only meet rigorous performance standards but also simplify the analytical process. This work explores the principles and methodology of CAC and presents case studies that demonstrate its practical applications in advancing chemical analysis towards more efficient method development and evaluation.

点击分析化学（CAC）是一种受点击化学原理启发的新方法，强调简单、高效和可靠。click化学革新了合成方法，而CAC旨在通过从不同角度提供方法评估框架来增强化学分析，重点是提高分析技术的实用性和适用性。在这项工作中，我们提出了点击分析化学指数（CACI）作为一个实用和用户友好的工具，为评估分析方法提供了度量和软件解决方案。该软件可以在bit.ly/CACI2025上以开源的形式获得。CACI系统允许在技术之间进行客观和公正的比较，鼓励开发在不牺牲性能的情况下更容易实现的方法。通过促进方法设计的简单性和实用性，CACI支持分析方法的开发，这些分析方法不仅符合严格的性能标准，而且简化了分析过程。这项工作探讨了CAC的原理和方法，并提出了案例研究，展示了其在推进化学分析方面的实际应用，以实现更有效的方法开发和评估。

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引用次数: 0

Polydopamine-graphene oxide aerogel for in-tube solid-phase microextraction of polycyclic aromatic hydrocarbons 多环芳烃管内固相微萃取用聚多巴胺-氧化石墨烯气凝胶

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2024.100144

Ziyi Jiang, Yanan Bu, Juanjuan Feng, Min Sun

Due to the wide distribution and potential carcinogenicity, teratogenicity and mutagenicity, polycyclic aromatic hydrocarbons (PAHs) have attracted much attention, requiring efficient and sensitive methods for detection. In order to improve the stability and extraction performance of graphene oxide aerogel, polydopamine was introduced to functionalize it. Polydopamine-hybridized graphene oxide aerogel was in-situ fabricated on the surface of titanium wire. The composite material was characterized by SEM and FT-IR. Three aerogel-coated wires were filled in a polyetheretherketone tube for in-tube solid-phase microextraction. Coupled with high performance liquid chromatography, the tube showed good extraction performance for several PAHs. Under the optimal conditions (sampling volume of 60 mL, sampling rate of 1.50 mL/min, sample pH of 7.3, 0.5 % (v/v) of methanol and 1.0 % (w/v) of NaCl in sample, desorption time of 1.0 min), an online analytical method was developed for determining trace PAHs from water samples, with low detection limits (0.01–0.05 μg/L), wide linear ranges (0.03–50 μg/L, 0.15–100 μg/L) with correlation coefficients (0.9953–0.9992) and satisfactory repeatability (RSDs, 0.22 %-4.42 % for intra-day, 1.42 %-5.18 % for inter-day). The method was applied to analyze some water samples including leaching solutions of coal ash and paper food box, some targets were found. The recoveries in these samples with different spiked levels (2.0 and 10.0 μg/L) were in the range of 81–117 %.

多环芳烃（polycyclic aromatic hydrocarbons, PAHs）由于分布广泛，具有潜在的致癌性、致畸性和诱变性，备受关注，需要高效、灵敏的检测方法。为了提高氧化石墨烯气凝胶的稳定性和提取性能，引入聚多巴胺对其进行功能化处理。在钛丝表面原位制备了聚多巴胺杂化氧化石墨烯气凝胶。采用SEM和FT-IR对复合材料进行了表征。将三根涂有气凝胶的金属丝填充在聚醚醚酮管中进行管内固相微萃取。结合高效液相色谱法，对几种多环芳烃的提取效果良好。在最佳条件下(进样量为60 mL，进样率为1.50 mL/min，样品pH为7.3，样品中甲醇用量为0.5% (v/v)， NaCl用量为1.0% (w/v)，解吸时间为1.0 min)，建立了水样中痕量多环芳烃的在线分析方法。该方法检出限低（0.01 ~ 0.05 μg/L），线性范围宽（0.03 ~ 50 μg/L, 0.15 ~ 100 μg/L），相关系数为0.9953 ~ 0.9992，重复性好（日内rsd为0.22% ~ 4.42%）；盘中1.42% - 5.18%)。应用该方法对煤灰浸出液和纸制食品盒等水样进行了分析，发现了一些指标。不同加标水平（2.0和10.0 μg/L）的加标回收率在81% ~ 117%之间。

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引用次数: 0

Nitrogen-rich covalent organic polymers for efficient solid phase extraction of nonsteroidal anti-inflammatory drugs from water samples 富氮共价有机聚合物用于高效固相萃取水样中非甾体抗炎药

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100148

Yuqi Cheng , Jia Li , Xiaochen Xiu , Xinghua Teng , Wen Zhang , Lei Ji , Leilei Wang

Non-steroidal anti-inflammatory drugs (NSAIDs) have received increasing attention owing to their ubiquitous occurrence in environmental water systems and adverse effects. In order to monitor trace levels of NSAIDs from complex water samples, development of facile and efficient sample pretreatment is of great significance. Herein, a nitrogen-rich covalent organic polymer containing phenyl, triazine and amine groups was fabricated via solvent-free copolymerization. Then, utilizing nitrogen-rich covalent organic polymer as adsorbent for solid phase extraction cartridges, the pretreatment method was combined with high-performance liquid chromatography-diode array detection to quantify five representative NSAIDs (ketoprofen, carprofen, flurbiprofen, diclofenac and mefenamic acid) in environmental water samples. Under the optimal extraction conditions (adsorbent amount: 40 mg; NaCl concentration: 0%; pH 6; extraction time: 20min; eluent solvent: 4 mL of formic acid/acetonitrile (5%, v/v)), the proposed method provided low detection limits (0.06–0.2 μg L^-1), wide linear ranges (0.2–100 μg L^-1) with correlation coefficients (0.9991–0.9997) and acceptable precision (RSDs, 6.6–8.5% for intra-day, 7.2–9.5% for inter-day). The practical application of the method was confirmed through the successful determination of NSAIDs in tap water, surface water, and sewage. The recoveries in these samples at the four NSAIDs concentration levels ranged from 81.3% to 109.8%, with the RSDs lower than 7.8%.

非甾体类抗炎药（NSAIDs）因其在环境水系统中的普遍存在和不良反应而受到越来越多的关注。为了监测复杂水样中痕量非甾体抗炎药的水平，开发简便、高效的样品预处理方法具有重要意义。本文采用无溶剂共聚法制备了含苯基、三嗪和胺基的富氮共价有机聚合物。然后，利用富氮共价有机聚合物作为固相萃取管的吸附剂，将预处理方法与高效液相色谱-二极管阵列检测相结合，对环境水样中5种具有代表性的非甾体抗炎药（酮洛芬、卡洛芬、氟比洛芬、双氯芬酸和甲氧胺酸）进行定量。在最佳提取条件下(吸附剂用量：40 mg；NaCl浓度：0%；pH值6;提取时间：20min；洗脱溶剂：甲酸/乙腈（5%,v/v） 4 mL)，方法检出限低（0.06 ~ 0.2 μg L-1），线性范围宽（0.2 ~ 100 μg L-1），相关系数为0.9991 ~ 0.9997，精密度可接受（rsd：日内6.6 ~ 8.5%，日内7.2 ~ 9.5%）。通过自来水、地表水和污水中非甾体抗炎药的成功测定，证实了该方法的实际应用。4种非甾体抗炎药浓度下的加样回收率为81.3% ~ 109.8%，rsd均小于7.8%。

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引用次数: 0

Determination of acylcarnitines in intact brain tumors using coated blade spray mass spectrometry (CBS-MS) 涂布叶片喷雾质谱法测定完整脑肿瘤中的酰基肉碱

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2024.100146

Joanna Bogusiewicz , Karol Jaroch , Jacek Furtak , Marcin Birski , Krystyna Soszyńska , Anna Majdańska , Agata Ryfa , Marek Harat , Barbara Bojko

Potential biomarkers of cancerous alterations could be selected by profiling a wide range of analytes. For this purpose, analytical platforms enabling detailed analysis of different biological matrices are applied. However, after biomarker selection, it is essential to shorten the analysis time as much as possible to speed up the diagnostic process. Therefore, this study aimed to optimize and test the coated blade spray mass spectrometry (CBS-MS) method in analyzing potential biomarkers in brain tumor studies: acylcarnitine. Meningiomas with different mutation statuses in NF2 were studied due to the relation of NF2 mutation with the higher risk of malignant transformation and multiple meningiomas. The application of CBS-MS enabled the determination of acetylcarnitine concentration (AC C2:0) and propionylcarnitine (AC C3:0) in intact tumor tissue. However, it would be necessary to enlarge the study group to confirm the conclusions on the concentration of these analytes in NF2 mutant and wild-type meningiomas. Apart from qualitative analysis, the simultaneous detection of a wide range of acylcarnitines in untargeted analysis was also possible.

癌症改变的潜在生物标志物可以通过分析广泛的分析物来选择。为此，应用了能够对不同生物基质进行详细分析的分析平台。然而，在生物标志物选择之后，必须尽可能缩短分析时间以加快诊断过程。因此，本研究旨在优化和测试涂层叶片喷雾质谱（CBS-MS）分析脑肿瘤研究中潜在生物标志物酰基肉碱的方法。由于NF2突变与恶性转化和多发性脑膜瘤的高风险相关，我们对不同突变状态的脑膜瘤进行了研究。应用CBS-MS可以测定完整肿瘤组织中乙酰肉碱（AC C2:0）和丙基肉碱（AC C3:0）的浓度。然而，有必要扩大研究小组，以证实NF2突变型和野生型脑膜瘤中这些分析物浓度的结论。除了定性分析外，还可以在非靶向分析中同时检测到大范围的酰基肉碱。

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引用次数: 0

Maximizing the neuroprotection from Citrus aurantium leaves: Optimization of a blended extract from a sequential extraction process with compressed fluids and NADES 最大限度地提高柑橘叶的神经保护作用：从压缩流体和NADES的顺序提取过程中优化混合提取物

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100149

Victor M. Amador-Luna, Miguel Herrero, Marta Jiménez de la Parra, Ángel Gómez Arribas, Elena Ibáñez, Lidia Montero

Citrus aurantium, also known as bitter orange, and the by-products obtained during its processing are a rich source of bioactive compounds. In particular, leaves from the tree pruning and from fruits harvesting are considered an agrifood-related waste with high valorization potential. Considering the wide variety of bioactive compounds present in the leaves (carotenoids, terpenes and phenolic compounds), this study is focused on the valorization of C. aurantium pruning waste through a sequential three-step extraction process using green extraction techniques, i.e. supercritical fluid extraction (SFE), followed by pressurized liquid extraction (PLE) using natural deep eutectic solvents (NADES), and an antisolvent extraction to recover the remaining bioactive compounds adsorbed to the NADES and extraction residues. In this sense, this is the first time that PLE using NADES followed by an antisolvent step to re-extract the compounds from the PLE residue is presented. Moreover, different protocols to efficiently remove the NADES from the PLE extract were also studied for the first time. Due to the different nature and bioactivity of the obtained extracts, the mixture of the three fractions was optimized to enhance its overall preventive potential against neurodegenerative diseases. Finally, its scalability to a semi-pilot scale was evaluated, giving rise to increased bioactive values of the blended extract.

金柑橘，也被称为苦橙，在其加工过程中获得的副产品是生物活性化合物的丰富来源。特别是，树木修剪和水果收获的叶子被认为是具有高增值潜力的农业食品相关废物。考虑到叶片中存在多种生物活性化合物（类胡萝卜素、萜烯和酚类化合物），本研究主要通过采用绿色萃取技术，即超临界流体萃取（SFE），然后使用天然深共晶溶剂（NADES）加压液体萃取（PLE），通过三步连续提取过程对金金莲剪枝废弃物进行价值化。以及反溶剂萃取以回收吸附在NADES和萃取残留物上的剩余生物活性化合物。从这个意义上说，这是第一次提出使用NADES和反溶剂步骤从PLE残留物中重新提取化合物的PLE。此外，我们还首次研究了不同的方法来有效地去除葡萄提取物中的NADES。由于所获得的提取物的不同性质和生物活性，优化了三个部分的混合物，以增强其对神经退行性疾病的整体预防潜力。最后，对其可扩展性进行了半中试规模评估，从而提高了混合提取物的生物活性值。

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引用次数: 0