Advances in Sample Preparation最新文献_第2页

Ionic liquid-grafted aminosilica-graphene oxide sorbent for efficient microextraction by packed sorbent of multiclass pesticides in wine 离子液体接枝氨基硅-氧化石墨烯吸附剂对葡萄酒中多类农药的高效微萃取

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-10-01 DOI: 10.1016/j.sampre.2025.100217

Alessandra Timóteo Cardoso , Gloria Domínguez-Rodríguez , Alejandro Cifuentes , Fernando Mauro Lanças

Monitoring pesticide residues in wine is essential for ensuring food safety, as these compounds and their metabolites can persist in the final product and pose potential health risks. This study reports the development of a hybrid sorbent based on graphene oxide anchored to aminosilica particles (GO@Si), functionalized with ionic liquids (ILs) via direct anion-exchange. Among the tested combinations, GO@Si-[VHIm]⁺PF₆⁻ exhibited the best extraction performance due to its multiple interaction mechanisms with analytes. This sorbent was integrated into a microextraction by packed sorbent (MEPS) system for the extraction of six multiclass pesticides from wine, followed by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) analysis. After optimizing extraction conditions using univariate and multivariate approaches, the method demonstrated excellent linearity (r² ≥ 0.9958), satisfactory precision (RSDs < 15 %), and recoveries ranging from 49 % to 112 %. Limits of quantification were from 0.030 to 0.130 ng mL⁻¹, with negligible matrix effects in white, red, and rosé wines. The method also presented notable green advantages, including device reusability (up to six cycles) and low solvent consumption (0.7 mL per extraction). Sustainability assessments using AGREEprep and BAGI yielded favourable scores (0.52 and 57.5, respectively). This pilot study provides a promising and environmentally conscious analytical approach for multiclass pesticide monitoring in wines, with potential for further development into routine analysis.

监测葡萄酒中的农药残留对确保食品安全至关重要，因为这些化合物及其代谢物可能持续存在于最终产品中，并构成潜在的健康风险。本研究报告了一种基于氧化石墨烯锚定到氨基二氧化硅颗粒（GO@Si）的混合吸附剂的开发，通过直接阴离子交换与离子液体（ILs）功能化。在测试的组合中，GO@Si-[VHIm]⁺PF₆⁻由于与被测物的多重作用机制，表现出最好的萃取性能。将该吸附剂集成到包装吸附剂（MEPS）微萃取系统中，用于从葡萄酒中提取6种多类农药，并进行高效液相色谱-串联质谱（HPLC-MS/MS）分析。采用单因素和多因素优化提取条件，结果表明，该方法线性度高（r²≥0.9958），精密度高（rsd = 15%），加样回收率为49% ~ 112%。定量限为0.030 ~ 0.130 ng mL（毒血症），在白、红、红葡萄酒中基质效应可以忽略不计。该方法还具有显著的绿色优势，包括设备可重复使用（多达6次循环）和低溶剂消耗（每次提取0.7 mL）。使用AGREEprep和BAGI的可持续性评估获得了有利的分数（分别为0.52和57.5）。本初步研究为葡萄酒中多种农药的监测提供了一种有前景的、环保的分析方法，并有进一步发展为常规分析的潜力。

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引用次数: 0

Introducing a modified sample preparation and straightforward elemental ratio determination strategy with LA-ICP-MS to expand the nanoparticle probing toolkit 引入改进的样品制备和直接元素比测定策略与LA-ICP-MS扩展纳米颗粒探测工具箱

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-10-01 DOI: 10.1016/j.sampre.2025.100223

Olga Lanaridi , Yan Chen , Jakob Nils Blaschke , Pablo Ayala , Bernhard C. Bayer , Dominik Eder , Andreas Limbeck

Nanoparticles (NPs) are employed in a wide range of applications due to some of their unique characteristics. Since their properties are partly determined by their composition, accurate determination of their stoichiometry is of paramount importance for optimization and fine tuning of their properties.

We propose a laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) procedure which enables determination of NP composition. Small NP quantities (approx. 1 mg) are dispersed in a polymeric solution which is then spin coated onto a Si wafer, thereby ensuring uniform distribution of the NPs within the thin polymer film deposited on the Si substrate. Matrix-matched standards are similarly prepared by mixing elemental aqueous stock solutions with the same polymer solution, followed by spin coating.

After thorough optimization of the sample preparation, and the parameters used for laser-ablation and subsequent ICP-MS analysis, the content of the analytes could be determined with a relative standard deviation (RSD) of < 2 % for standards and < 3–8 % for the NP samples, depending on the NP type, with detection limits lower than 0.2000 µg/g for all elements. Based on the results determined for the individual NP constituents, prevailing elemental ratios have been assessed.

Yttria-doped zirconia of known stoichiometry, i.e., (ZrO₂)_0.98(Y₂O₃)_0.08, was used as a reference material to validate the fit of the developed approach for the stoichiometric determination of NPs. The experimentally determined stoichiometry is in agreement with the one provided by the manufacturer. The applicability of the method is further demonstrated by assessment of the loading of CdS rods with medium-entropy (CoNiMoW)S NPs, which are interesting as novel catalysts and stoichiometric determination of Zr-based metal organic frameworks (MOFs), which function as catalysts in CO₂ reduction.

纳米粒子（NPs）由于其一些独特的特性而被广泛应用。由于它们的性质部分是由它们的组成决定的，因此准确测定它们的化学计量对于优化和微调它们的性质至关重要。我们提出了一种激光烧蚀-电感耦合等离子体质谱（LA-ICP-MS）程序，可以确定NP组成。小的NP数量(大约。1毫克)分散在聚合物溶液中，然后自旋涂覆在硅晶片上，从而确保NPs在沉积在硅衬底上的薄聚合物薄膜内均匀分布。基质匹配的标准品同样是通过将元素水原液与相同的聚合物溶液混合，然后进行旋转涂层来制备的。经过对样品制备、激光烧蚀及后续ICP-MS分析参数的全面优化，根据NP类型，标准样品的相对标准偏差（RSD）为2%，NP样品的相对标准偏差（RSD）为3 - 8%，所有元素的检出限均低于0.2000µg/g。根据对单个NP成分确定的结果，评估了普遍的元素比率。以已知化学计量的氧化锆（ZrO2）0.98(Y2O3)0.08作为对照物质，验证了该方法测定NPs化学计量的拟合性。实验测定的化学计量与厂家提供的一致。该方法的适用性通过评估具有中熵（CoNiMoW）S NPs的CdS棒的负载以及化学计量学测定作为CO2还原催化剂的zr基金属有机框架（mof）进一步得到验证。

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引用次数: 0

From lemon peels to bioactive peptides: protein recovery by pressurized liquid extraction and hydrolysates characterization by UHPLC-ESI-QTOF-MS/MS 从柠檬皮到生物活性肽：加压液体萃取法提取蛋白质和UHPLC-ESI-QTOF-MS/MS表征水解产物

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-10-01 DOI: 10.1016/j.sampre.2025.100218

Esther Gómez-Mejía , María Concepción García , María Castro-Puyana , María Luisa Marina

This study aimed to develop a sustainable and efficient method for protein recovery from lemon peels using Pressurized Liquid Extraction (PLE), optimized through experimental design and response surface methodology. The final protocol, employing 18 % (v/v) ethanol, 110 °C, and a 7-min extraction time, demonstrated high extraction efficiency (66 %) and environmental compatibility, achieving a greenness score of 0.59 (AGREEprep). The optimized protein extract was subsequently hydrolyzed using alcalase and thermolysin, and the resulting peptide fractions were characterized by spectrophotometric methods and by Ultra High-Performance Liquid Chromatography coupled to Electrospray Ionization Quadrupole Time-of-Flight Mass Spectrometry (UHPLC-ESI-QTOF-MS/MS). A total of 58 peptides were identified, 39 of which originated from lemon proteins, along with 19 polyphenols, such as vicenin-2, narirutin or subaphylin, and other compounds (e.g., organic acids, amino acids, and purine nucleosides), revealing a diverse and multifunctional bioactive profile. Bioactivity assays demonstrated that the thermolysin hydrolysate exhibited the highest antioxidant (97 ± 1 % inhibition of hydroxyl radicals), antimicrobial (MIC = 0.75 mg/mL against Staphylococcus aureus), and antihypertensive activities (49 ± 3 % angiotensin-converting enzyme inhibition), likely due to the presence of peptides enriched in aromatic amino acids such as phenylalanine and tyrosine.

本研究旨在建立一种可持续、高效的从柠檬皮中提取蛋白质的加压液体萃取方法，并通过实验设计和响应面法对其进行优化。最终方案采用18% （v/v）乙醇，110°C，提取时间为7 min，具有较高的提取效率（66%）和环境相容性，绿色评分为0.59 （AGREEprep）。利用alcalase和thermolysin对优化后的蛋白提取物进行水解，并通过分光光度法和超高效液相色谱-电喷雾电离四极杆飞行时间质谱联用（UHPLC-ESI-QTOF-MS/MS）对所得到的肽段进行表征。共鉴定出58个多肽，其中39个来自柠檬蛋白，以及19种多酚，如vicenin-2、narirutin或subaphylin，以及其他化合物（如有机酸、氨基酸和嘌呤核苷），揭示了多样化和多功能的生物活性谱。生物活性分析表明，热溶菌素水解产物具有最高的抗氧化活性（97±1%的羟基自由基抑制），抗菌活性（对金黄色葡萄球菌的MIC = 0.75 mg/mL）和降压活性（49±3%的血管紧张素转换酶抑制），这可能是由于富含苯基丙氨酸和酪氨酸等芳香族氨基酸的肽的存在。

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引用次数: 0

Recent progress in solid- and liquid-phase microextraction methods for the extraction and quantification of current-use pesticides 固体微萃取法和液相微萃取法用于农药提取和定量的研究进展

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-10-01 DOI: 10.1016/j.sampre.2025.100215

Seyedeh Bentolhoda Hosseinian , Milad Ghani , Jahan Bakhsh Raoof

The widespread use of pesticides has led to their pervasive presence in diverse environmental matrices such as water, air, and soil. Therefore, accurate and reliable determination of pesticides in various sample types is essential. In recent years, a range of miniaturized extraction techniques, particularly solid-phase microextraction (SPME) and liquid-phase microextraction (LPME), have been developed. This review provides a comprehensive overview of recent advancements in liquid- and solid-phase microextraction techniques for separation and quantification of pesticides, while also critically evaluating their respective advantages and limitations. In addition, different configurations of solid- and liquid phase microextraction used for the extraction of pesticides are discussed. Moreover, various advanced materials such as molecularly imprinted polymers (MIPs), metal–organic frameworks (MOFs), 3D printed devices, Mxenes, and biopolymers used for the microextraction of pesticides were also discussed.

农药的广泛使用导致它们普遍存在于各种环境基质中，如水、空气和土壤。因此，准确、可靠地测定各种样品类型中的农药至关重要。近年来，以固相微萃取（SPME）和液相微萃取（LPME）为代表的一系列小型化萃取技术得到了发展。本文综述了用于农药分离和定量的液相微萃取和固相微萃取技术的最新进展，并对其各自的优点和局限性进行了批判性评价。此外，还讨论了用于农药提取的固、液相微萃取的不同配置。此外，还讨论了用于农药微提取的各种先进材料，如分子印迹聚合物（MIPs），金属有机框架（MOFs）， 3D打印设备，Mxenes和生物聚合物。

引用次数: 0

Optimization and enzymatic intensification of bioactive compound extraction from carob pulps with potential weight management applications 具有体重管理应用潜力的角豆粕生物活性化合物提取优化及酶促强化

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-10-01 DOI: 10.1016/j.sampre.2025.100219

Iván Benito-Vázquez , Manuel Garrido-Romero , Gema Hontoria-Caballo , Marina Díez-Municio , Francisco Javier Moreno , Ignacio Jiménez-Amezcua

Carob pulps (Ceratonia siliqua L.) are a rich source of bioactive compounds with potential benefits for weight management, particularly inositols, flavonoids and phenolic acids (e.g. gallic acid). This study aimed to develop and optimize a sustainable extraction method to maximize the recovery of these target compounds. A solid–liquid extraction (SLE) was first optimized using a Box–Behnken experimental design, evaluating different variables (temperature, time, sample concentration and ethanol content). A two-variable (2 V) model focused on the extraction of inositols and gallic acid was identified as the most efficient allowing high extraction yields (45 °C, 28 min, 100 mg/mL, pure water) compared to the three-variable (3 V) model (90 ºC, 42 min, 100 mg/mL, ethanol 50 %), which additionally prioritized the extraction of flavonoids. To further intensify the extraction, enzyme-assisted extraction (EAE) using two commercial cellulases were studied and significantly enhanced gallic acid release (up to 2.39 mg/g), confirming its selective extraction from the plant matrix. A two-step strategy combining EAE under 2 V conditions (inositols and gallic acid) with a second cycle of 3 V SLE (flavonoids) was selected as an ecofriendly alternative to maximize the content of bioactives and applied on different carob samples. Pinitol was the most abundant compound across all samples (16.7–73.0 mg/g) and gallic acid also achieved high values (1.9–8.4 mg/g). Regarding flavonoids, kaempferol and luteolin glucosides were the most abundant. This study provides a comprehensive framework for efficient and sustainable sample preparation of carob-derived bioactives intended for functional food or nutraceutical applications targeting weight management.

角豆浆（Ceratonia silqua L.）富含生物活性化合物，对体重管理有潜在的好处，特别是肌醇、类黄酮和酚酸（如没食子酸）。本研究旨在开发和优化一种可持续的提取方法，以最大限度地提高这些目标化合物的回收率。首先采用Box-Behnken实验设计，对不同的变量（温度、时间、样品浓度和乙醇含量）进行优化。与三变量（3 V）模型（90℃，42 min, 100 mg/mL，乙醇50%）相比，专注于提取肌醇和没食子酸的双变量（2 V）模型效率最高，提取率高（45°C, 28 min, 100 mg/mL，纯水），其中黄酮类化合物的提取更为优先。为了进一步加强提取，研究了两种商用纤维素酶的酶辅助提取（EAE），显著提高了没食子酸的释放（高达2.39 mg/g），证实了没食子酸从植物基质中的选择性提取。选择2 V条件下（肌醇和没食子酸）EAE与2 V条件下（黄酮类化合物）SLE相结合的两步策略作为最大限度地提高生物活性含量的生态替代方案，并应用于不同的角豆样品。蒎醇是所有样品中含量最高的化合物（16.7 ~ 73.0 mg/g），没食子酸也达到了很高的含量（1.9 ~ 8.4 mg/g）。黄酮类化合物以山奈酚和木犀草素苷含量最多。本研究为有效和可持续的碳水化合物衍生生物活性物质的样品制备提供了一个全面的框架，用于功能食品或营养保健应用，以控制体重。

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引用次数: 0

In-house metal-organic framework material for stir-bar sorptive extraction of acidic pharmaceutical compounds from environmental water samples 用于搅拌棒吸附萃取环境水样中酸性药物化合物的内部金属有机框架材料

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-10-01 DOI: 10.1016/j.sampre.2025.100224

Abril Trullàs , Héctor Martínez-Pérez-Cejuela , Francesc Borrull , Mónica Catalá-Icardo , José Manuel Herrero-Martínez , Rosa Maria Marcé , Núria Fontanals

Pharmaceutical residues are increasingly recognized as emerging contaminants in aquatic environments due to their widespread consumption, improper disposal, and insufficient removal in wastewater treatment plants. These compounds, often found at trace levels, pose ecological risks owing to their bioaccumulation potential and biological activity. Micro-extraction techniques, especially stir-bar sorptive extraction (SBSE), have gained widespread use for their effectiveness in preconcentration and analytical applications. However, commercial SBSE coatings show limited retention of polar analytes and suffer from poor mechanical stability as well as high purchase cost. To address these limitations, this study presents the development and evaluation of an in-house hybrid coating material for SBSE with a total cost <5€/unit, based on metal-organic frameworks (MOFs) functionalized with amine groups that provide weak anion exchange (WAX) interactions. The performance of the amino-functionalized MOF attached to a glycidyl methacrylate-based monolith (GMA@NH₂-UiO-66(Zr)) was assessed for the extraction of acidic pharmaceutical compounds from environmental water samples, followed by determination using liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the proper optimization, good analytical figures were obtained for river water samples, including the method’s limits of detection as low as 2 ng/L, adequate recoveries (22–41 %), matrix effect between +9 and -2 % and acceptable precision expressed as relative standard deviation below 25 %. Once validated, the method was applied for the determination of acidic pharmaceuticals from environmental water samples, which were found at ng/L level. The new material exhibited improved retention of polar pharmaceuticals, high stability, and reproducibility, demonstrating its potential as an effective tool for environmental monitoring of pharmaceutical contaminants.

由于药物残留的广泛使用、处置不当和废水处理厂去除不足，它们越来越被认为是水生环境中的新兴污染物。这些化合物通常以微量水平发现，由于其生物蓄积潜力和生物活性而构成生态风险。微萃取技术，特别是搅拌棒吸附萃取（SBSE），因其在富集和分析方面的有效性而得到了广泛的应用。然而，商用SBSE涂料显示极性分析物的保留有限，机械稳定性差，购买成本高。为了解决这些限制，本研究提出了一种用于SBSE的内部混合涂层材料的开发和评估，总成本为5欧元/单位，该材料基于具有弱阴离子交换（WAX）相互作用的胺基功能化的金属有机框架（MOFs）。采用液相色谱-串联质谱（LC-MS/MS）分析了氨基功能化MOF对环境水样中酸性药物的萃取性能，并对其与甲基丙烯酸缩水甘油酯基单体（GMA@NH₂- uui -66(Zr)）的吸附性能进行了评价。经过适当的优化，获得了良好的分析数据，包括方法的检出限低至2 ng/L，适当的回收率（22 - 41%），矩阵效应在+9 ~ - 2%之间，可接受的精密度表示为相对标准偏差低于25%。验证后，该方法可用于环境水样中酸性药物的测定，其含量为ng/L。新材料表现出极性药物保留率的提高，稳定性和可重复性高，表明其作为药物污染物环境监测的有效工具的潜力。

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引用次数: 0

Chicken egg white coated paper, a sustainable mixed-mode cationic exchange biocomposite to extract antidepressants from saliva samples prior to their determination by direct infusion mass spectrometry 鸡蛋清涂布纸是一种可持续的混合模式阳离子交换生物复合材料，用于直接输注质谱法测定唾液样品中的抗抑郁药物

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-10-01 DOI: 10.1016/j.sampre.2025.100226

Ana M. Pedraza-Soto, Rafael Lucena, Soledad Cárdenas

Proteinaceous materials are useful precursors for preparing sustainable and cost-effective sorptive phases. Among them, chicken egg white is an excellent alternative, serving as a source of ovalbumin that can be used as a biosorbent. In this article, the combination of egg white with cellulose paper is evaluated to synthesize a planar protein-based sorptive phase with high porosity and surface area. For this purpose, the paper was dip-coated in egg-white, followed by thermal curing that induced protein denaturation and self-crosslinking. The preparation was quite simple and affordable, since it did not require subsequent functionalization procedures, allowing the preparation of 25 sorptive phases with only 1 mL of pasteurized egg white. The resulting egg-white paper (EW-paper) enabled the isolation of the analytes through a mixed-mode interaction mechanism, comprising both hydrophobic and cation-exchange interactions. This potential was corroborated by evaluating the extraction capacity of the EW-paper towards some selective serotonin reuptake inhibitors (SSRI) (fluoxetine, paroxetine, sertraline, and venlafaxine) from saliva samples. The analytes were finally determined by direct infusion mass spectrometry analysis. Once optimized, the method allows the determination of the target compounds in the low µgL^-1 range, also fulfilling the validation criteria in terms of precision (better than 9.1 % and 11.8 % in intra- and inter-day precision, respectively) and accuracy (in the range 84 -118 %). Finally, the applicability of the method was demonstrated by analyzing real saliva samples from a patient under paroxetine treatment.

蛋白质材料是制备可持续和具有成本效益的吸附相的有用前体。其中，蛋清是一个很好的替代品，作为卵白蛋白的来源，可以用作生物吸附剂。本文研究了蛋清与纤维素纸的结合，合成了一种具有高孔隙率和高表面积的平面蛋白基吸附相。为此，将纸浸在蛋白中，然后进行热固化，诱导蛋白质变性和自交联。该制备非常简单且价格合理，因为它不需要后续的功能化程序，仅用1ml巴氏灭菌的蛋清即可制备25个吸附相。由此产生的蛋清纸（EW-paper）通过混合模式相互作用机制（包括疏水和阳离子交换相互作用）分离分析物。通过评估ew论文对唾液样本中一些选择性血清素再摄取抑制剂（氟西汀、帕罗西汀、舍曲林和文拉法辛）的提取能力，证实了这一潜力。最后用直接输注质谱法测定分析物。优化后，该方法可在低µgL-1范围内测定目标化合物，精密度（日内精密度分别优于9.1%和11.8%）和准确度（范围为84 - 118%）均满足验证标准。最后，通过分析帕罗西汀治疗患者的真实唾液样本，证明了该方法的适用性。

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引用次数: 0

Green metric for microwave-assisted sample preparation for elemental analysis: GreenPrep MW Score 用于元素分析的微波辅助样品制备的绿色度量：GreenPrep MW评分

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-10-01 DOI: 10.1016/j.sampre.2025.100216

Joaquim A. Nóbrega , Lorenzo Rossi , Gianpaolo Rota , Mirco Rossetti , Valentina Carrara , Camillo Pirola , Giulio Colnaghi , Diego Carnaroglio

Rapidly moving to the 3^rd decade of the 21^st century, it is clear that our technologies must evolve to sustainable processes, not aggressive to the environment nor to all forms of life. Chemical sciences are going green and surely analytical chemistry is moving towards this same direction. But we need to speed up the pace. To evaluate an analytical procedure, we should be able to validate it. Nowadays, method validation is not only the demonstration that analytical results are accurate, in fact method validation is also related to green chemistry aspects. If we think about elemental analysis, we can state that the sample preparation step has been improved, nonetheless it certainly requires further improvements through the development of greener procedures. In this contribution, we propose a set of green metrics named GreenPrep MW Score for the evaluation of microwave-assisted sample preparation procedures using different technologies, either based on cavity microwave oven, or on a single reaction chamber system. The GreenPrep MW Score was proposed considering the whole analytical procedure and how chemical parameters, technology variables and workflow can be optimized, and how these factors impact green metrics score. The authors do not intend to substitute sound metrics already proposed for evaluating the sample preparation step. Our goal is to propose a complementary strategy which helps us identify specific points to be improved in microwave-assisted procedures. The application of the developed metric was demonstrated for several samples containing different matrices, such as foods, multivitamin tablets, spodumene; in addition, strategies for improving green chemistry aspects were discussed.

迅速进入21世纪的第三个十年，很明显，我们的技术必须发展到可持续的进程，而不是对环境和所有形式的生命造成破坏。化学科学正在走向绿色，毫无疑问，分析化学也在朝着同样的方向发展。但我们需要加快步伐。为了评估一个分析程序，我们应该能够验证它。如今，方法验证不仅仅是证明分析结果的准确性，事实上，方法验证还涉及到绿色化学的各个方面。如果我们考虑元素分析，我们可以说样品制备步骤已经改进，尽管如此，它肯定需要通过开发更环保的程序进一步改进。在这篇文章中，我们提出了一套绿色指标，称为GreenPrep MW Score，用于评估使用不同技术的微波辅助样品制备程序，无论是基于空腔微波炉还是单一反应室系统。GreenPrep MW评分的提出考虑了整个分析过程，以及如何优化化学参数、技术变量和工作流程，以及这些因素如何影响绿色指标评分。作者不打算取代已经提出的评估样品制备步骤的健全指标。我们的目标是提出一种补充策略，帮助我们确定微波辅助手术中需要改进的具体点。该方法应用于几种含有不同基质的样品，如食品、复合维生素片、锂辉石；此外，还讨论了绿色化学方面的改进策略。

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引用次数: 0

Polyhedral oligomeric silsesquioxane hybrid monolithic microcartridges for the determination of β-lactoglobulin in food by on-line solid-phase extraction capillary electrophoresis-mass spectrometry 在线固相萃取-毛细管电泳-质谱联用测定食品中β-乳球蛋白的多面体低聚硅氧烷杂化整体微盒

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-10-01 DOI: 10.1016/j.sampre.2025.100220

Renan Vitek , Tahereh Tehrani , Laura Pont , María Vergara-Barberán , José Manuel Herrero-Martínez , Fernando Benavente , Jorge C. Masini

A novel polyhedral oligomeric silsesquioxane methacryl substituted (POSS-MA) monolithic microcartridge was prepared for the determination of low levels of the allergenic protein β-lactoglobulin (β-LG) in food by on-line solid-phase extraction capillary electrophoresis-mass spectrometry (SPE-CE-MS). The material was synthesized inside a 250 μm inner diameter (i.d.) capillary column by free radical polymerization using a simple "one-pot" method. This capillary column was subsequently cut and straightforwardly assembled as microcartridges connected in-line with 75 μm i.d. separation capillaries for SPE-CE-MS. Several SPE-CE-MS parameters (such as loading time, type of eluent, or time and pressure of elution) were optimized using an acidic background electrolyte (BGE) composed of 2 M acetic acid (HAc, pH 2.2). Under optimized conditions, the protein sample was loaded at 930 mbar for 20 min (ca. 110 μL), followed by a washing step with BGE at 930 mbar for 1 min, and finally eluted with 2 M HAc in methanol at 100 mbar for 60 s (ca. 600 nL). The method exhibited linearity from 0.25 to 10 μg·mL⁻¹ of β-LG, with a limit of detection of 0.1 μg·mL⁻¹, and a 100-fold increase in sensitivity compared to CE-MS. It was successfully applied to the determination of β-LG in dairy free white breads, yielding satisfactory results. These outcomes highlight the strong potential of the developed SPE-CE-MS method, using plug-and-play POSS-MA monolithic microcartridges, for precise food safety and quality control.

采用在线固相萃取-毛细管电泳-质谱联用技术（SPE-CE-MS）制备了一种新型多面体低聚硅氧烷甲基丙烯酸取代（POSS-MA）单片微瓶，用于食品中低含量致敏蛋白β-乳球蛋白（β-LG）的检测。在内径为250 μm （i.d）的毛细管柱内，采用简单的“一锅法”，采用自由基聚合法制备了该材料。该毛细管柱随后被切割并直接组装成与75 μm id分离毛细管直线连接的微盒，用于SPE-CE-MS。采用由2 M乙酸（HAc, pH 2.2）组成的酸性背景电解质（BGE），优化了SPE-CE-MS的几个参数（如上样时间、洗脱液类型或洗脱时间和压力）。在优化后的条件下，蛋白样品在930 mbar下负载20 min（约110 μL），然后用BGE在930 mbar下洗涤1 min，最后用2 M HAc在100 mbar的甲醇中洗脱60 s（约600 nL）。该方法在β-LG浓度0.25 ~ 10 μg·mL−1范围内呈线性关系，检出限为0.1 μg·mL−1，灵敏度比CE-MS提高100倍。该法成功地应用于无乳白面包中β-LG的测定，结果令人满意。这些结果突出了开发的SPE-CE-MS方法的强大潜力，该方法使用即插即用的POSS-MA单片微盒，用于精确的食品安全和质量控制。

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引用次数: 0

Comparison of biodegradable polycaprolactone nanofibers and synthetic polyamide nanofibers as a novel, sustainable sorbent for a spin filter microextraction of xenobiotics from river water 生物可降解聚己内酯纳米纤维与合成聚酰胺纳米纤维在自旋过滤器微萃取河水中异种生物中的吸附效果比较

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-09-16 DOI: 10.1016/j.sampre.2025.100214

Ewelina Czyz , Karolína Macháčková , Jakub Erben , Pavel Holec , František Švec , Dalibor Šatínský

We evaluated the application of nanofibers made from different biodegradable and synthetic polymers as sorbents in a new technique of spin filter fiber-microextraction. Biodegradable polycaprolactone fibers, produced via the meltblowing process exhibited robust hydrophobic interactions with lipophilic analytes and were the most effective. The highly porous and permeable structure of the fibrous material ensured exhaustive extraction of xenobiotics from river water. Recovery rates ranged from 81.8 to 105.2 %, except for 4-nitrophenol, a more polar analyte, for which the recovery was 60 %. Only 10 s were needed for activation, extraction, and elution, significantly reducing the time required to complete the procedure in only 30 s per sample. Our method exhibited excellent analytical performance, achieving linearity in the range of 50–2000 µg L⁻¹ for most analytes (100–2000 µg L⁻¹ for PNP and 2-CP; and 100–1000 µg L⁻¹ for PER) with a coefficient of determination (R²) greater than 0.9952. The limits of detection were recalculated based on the slope of the calibration curves and the standard deviation of six replicate measurements at the lowest calibration point for each analyte, yielding values in the range of 7.0–36.6 µgL^-1. Repeatability between extractions (i.e. inter-extraction precision) was evaluated by performing six parallel runs using different cartridges (n = 6). The obtained RSD precision values ranged from 2.2 to 3.3 % demonstrating the excellent uniformity of the nanofibrous materials filled in the devices . We also assessed the reusability of the individual cartridges by performing six consecutive extractions on the same spin filter (i.e. intra-cartridge precision, n = 6), yielding RSD values between 1.1 and 3.6 %. These results confirm that the spin filters cartridges filled with polycaprolactone nanofibers can be effectively reused for multiple extractions in absence of sample carry-over effect.

研究了由不同生物可降解聚合物和合成聚合物制成的纳米纤维作为吸附剂在自旋过滤纤维微萃取新技术中的应用。通过熔吹工艺生产的可生物降解聚己内酯纤维与亲脂分析物表现出强大的疏水相互作用，并且是最有效的。纤维材料的高度多孔性和渗透性结构确保了从河水中彻底提取异种生物。除极性较强的4-硝基苯酚的回收率为60%外，回收率为81.8% ~ 105.2%。活化、提取和洗脱只需要10秒，大大减少了完成每个样品仅需30秒的时间。我们的方法具有良好的分析性能，大多数分析物在50-2000µg L -⁻¹范围内呈线性（PNP和2-CP为100-2000µg L -⁻¹；PER为100-1000µg L -⁻），决定系数（R2）大于0.9952。根据校准曲线的斜率和每种分析物在最低校准点的6次重复测量的标准差重新计算检出限，得到的值范围为7.0-36.6µgL-1。通过使用不同的萃取盒（n = 6）进行6次平行运行来评估萃取之间的重复性（即萃取间的精密度）。得到的RSD精度值在2.2 ~ 3.3%之间，表明填充在器件中的纳米纤维材料具有良好的均匀性。我们还通过在相同的旋转过滤器上进行六次连续提取（即盒内精度，n = 6）来评估单个墨盒的可重复使用性，产生的RSD值在1.1到3.6%之间。这些结果证实了填充聚己内酯纳米纤维的自旋过滤器可以有效地重复使用多次提取，没有样品携带效应。

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