Advances in Sample Preparation最新文献_第3页

Recovery of proteins and bioactive compounds from turmeric (Curcuma longa) and ginger (Zingibber officinale) wastes using sustainable extraction techniques. Tentative identification of main extracted compounds by UHPLC-Q-TOF-MS/MS 利用可持续提取技术从姜黄（Curcuma longa）和姜（Zingibber officinale）废料中回收蛋白质和生物活性化合物。UHPLC-Q-TOF-MS/MS对主要提取物进行初步鉴定

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-09-13 DOI: 10.1016/j.sampre.2025.100213

Rubio-Marín Carlos , María Luisa Marina , María Concepción García

Ginger and turmeric are spices increasingly employed in juice production due to their outstanding composition and health benefits. This practice results in wastes that, like whole spices, likely constitute a cheap and sustainable source of proteins, as well as antioxidant and antimicrobial compounds, whose recovery has not yet been proposed. This work aims to evaluate low environmental impact techniques to make the most of these wastes: high-intensity focused ultrasounds (HIFU), subcritical water extraction (SWE), and enzyme-assisted extraction (EAE). In all cases, water was used as extracting solvent and experimental design chemometric tools (Box-Behnken and factorial 3² design) were employed to maximize the recovery of proteins, antioxidants, and antimicrobial compounds, while minimizing the formation of potentially harmful Maillard products during extraction. HIFU demonstrated a greater capability for extracting proteins, which increased significantly when combined with EAE using a polysaccharidase enzyme. The largest protein extraction was achieved from the ginger extract using HIFU for 18 min, at 60 ºC and 80 % amplitude, combined with EAE using Celluclast enzyme. The extracts obtained using SWE showed significant antioxidant activity, with a slight improvement observed when using 2 cycles instead of one. The highest antioxidant activity was observed in the extract obtained from the turmeric waste using SWE at 175 ºC for 15 min. The extracts also exhibited antimicrobial activity, especially against Staphylococcus aureus, highlighting the minimum inhibitory concentration obtained from the turmeric waste extract using SWE at 155 ºC for 9 min (0.15 mg/mL). The extracts showing the highest antioxidant or antimicrobial activity were analyzed by ultrahigh-performance liquid chromatography coupled to high-resolution tandem mass spectrometry for the tentative identification of main compounds responsible for the observed activities. Phenolic compounds, such as 6-gingerol and its derivatives in ginger waste extracts, and curcuminoids in turmeric waste extracts, were tentatively identified as the predominant constituents.

生姜和姜黄由于其出色的成分和健康益处而越来越多地用于果汁生产。这种做法产生的废物，就像整个香料一样，可能构成廉价和可持续的蛋白质来源，以及抗氧化和抗菌化合物，其回收尚未提出。这项工作旨在评估低环境影响技术，以充分利用这些废物：高强度聚焦超声（HIFU）、亚临界水提取（SWE）和酶辅助提取（EAE）。在所有情况下，均使用水作为提取溶剂，并采用实验设计化学测量工具（Box-Behnken和析因32设计）来最大限度地回收蛋白质、抗氧化剂和抗菌化合物，同时最大限度地减少提取过程中潜在有害美拉德产物的形成。HIFU显示出更大的蛋白质提取能力，当使用多糖酶与EAE联合使用时，蛋白质提取能力显著提高。在60ºC和80%振幅下，HIFU作用18 min，结合使用Celluclast酶的EAE，从姜提取物中提取的蛋白质最多。SWE提取的提取物具有显著的抗氧化活性，当使用2个周期而不是1个周期时，其抗氧化活性略有提高。从姜黄废料中提取的抗氧化活性最高，SWE在175℃下加热15 min。该提取物还显示出抗菌活性，特别是对金黄色葡萄球菌，突出显示姜黄废物提取物在155ºC下使用SWE处理9分钟（0.15 mg/mL）获得的最低抑制浓度。采用高效液相色谱联用高分辨率串联质谱法对抗氧化或抗菌活性最高的提取物进行了分析，初步确定了主要活性成分。初步确定了生姜提取物中的6-姜辣素及其衍生物和姜黄素等酚类化合物为主要成分。

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引用次数: 0

Versatile sorbent materials in sample preparation: Where do we go next? 样品制备中的多功能吸附材料：我们下一步要做什么？

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-09-04 DOI: 10.1016/j.sampre.2025.100211

Rafael Oliveira Martins, Maria Flávia Assunção Magalhães, Winnie Evelyn Valeria Perez Vite, Jussara da Silva Alves, Camila Will, Fernando Mauro Lanças

Continuous advances in sample preparation methods have led to the development of enhanced strategies to address the complexity of diverse matrices in both qualitative and quantitative analyses. These methods are designed to facilitate sample clean-up and preconcentration of target analytes before analysis by different analytical instruments. In both conventional and miniaturized solid-based approaches, the analytical performance of the extraction is primarily influenced by the sorbent phase. As the sorbent is responsible for mediating the interaction between the target analytes and the extraction material, careful selection is essential. In this context, a wide range of sorbent materials has been introduced to ensure efficient and selective interactions, supporting their application in sample preparation protocols. Nevertheless, the literature still lacks comprehensive and up-to-date reviews that highlight recent advances in sorbent development, including both conventional and bio-based alternatives. Therefore, this review aims to provide a current overview of sorbent innovations, discuss emerging trends, and outline potential future directions in the field.

样品制备方法的不断进步导致了增强策略的发展，以解决定性和定量分析中不同矩阵的复杂性。这些方法的目的是在不同的分析仪器分析之前，方便样品的清理和目标分析物的预浓缩。在传统和小型固体基方法中，萃取的分析性能主要受吸附相的影响。由于吸附剂负责调节目标分析物和萃取物质之间的相互作用，因此仔细选择是必不可少的。在这种情况下，广泛的吸附剂材料已经被引入，以确保有效和选择性的相互作用，支持它们在样品制备方案中的应用。然而，文献仍然缺乏全面和最新的评论，强调吸附剂发展的最新进展，包括传统和生物基替代品。因此，本综述旨在提供吸附剂创新的当前概述，讨论新兴趋势，并概述该领域潜在的未来方向。

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引用次数: 0

Investigating the impact of novel brominated flame retardants (NBFRs) on metabolite and nutritional profiles in aquatic organisms by in vivo solid-phase microextraction (SPME) 利用体内固相微萃取（SPME）技术研究新型溴化阻燃剂对水生生物代谢物和营养成分的影响

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-09-04 DOI: 10.1016/j.sampre.2025.100212

Tianning Chen , Pengfei Ye , Chen Yuan , Ling Fang , Nan Li , Guosheng Chen , Junlang Qiu , Fang Zhu , Gangfeng Ouyang

Novel brominated flame retardants (NBFRs), due to their ubiquitous environmental distribution in aquatic ecosystems and potential adverse effects to aquatic biota, have initiated global concerns. NBFRs were absorbed and bioaccumulated into aquatic organisms, impairing their growth while significantly disrupting metabolic and nutritional profiles deserves further elucidation, especially for in vivo and in situ characterization. In this study, we selected tilapia (Oreochromis mossambicus) as a model and developed an innovative in vivo sampling method using solid-phase microextraction (SPME) with a cationic covalent organic framework (COF) coating fiber, coupled with high performance liquid chromatography-electrospray ionization-Orbitrap mass spectrometry (HPLC-ESI-Orbitrap-MS) analysis. Our results demonstrated that self-made SPME fibers possessed excellent broad-spectrum extraction ability (totally 5250 molecular features were detected), and the developed analysis method has the advantages of greenness. SPME technology based on our self-made fiber was successfully applied in research of the impacts of NBFRs on tilapia. After statistical analysis, a total of 811 metabolites exhibited significant differential expression, including the nutritional components such as amino acids, glycosides, and lipids, which resulted in a decline in nutritional quality. These findings provided a new perspective for evaluating the ecological risk assessment of NBFRs, nutritional quality assessment of aquatic organisms and securing fishery products.

新型溴化阻燃剂（NBFRs）由于其在水生生态系统中普遍存在的环境分布和对水生生物群的潜在不利影响，引起了全球的关注。nfrs被吸收并积累到水生生物中，损害了它们的生长，同时显著破坏了它们的代谢和营养特征，值得进一步阐明，特别是在体内和原位表征方面。本研究以罗非鱼（Oreochromis mossambicus）为研究对象，采用阳离子共价有机骨架（COF）涂层纤维固相微萃取（SPME），结合高效液相色谱-电喷雾电离-轨道阱质谱（HPLC-ESI-Orbitrap-MS）分析，建立了一种创新的体内取样方法。结果表明，自制SPME纤维具有优异的广谱提取能力（共检测到5250个分子特征），所建立的分析方法具有绿色环保的优点。基于自制纤维的SPME技术成功应用于nfrs对罗非鱼的影响研究。经统计分析，共有811种代谢物表现出显著的差异表达，包括氨基酸、糖苷、脂类等营养成分，导致营养品质下降。这些发现为nfrs生态风险评价、水生生物营养质量评价和水产品安全提供了新的视角。

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引用次数: 0

In-situ simultaneous extraction of non-steroidal anti-inflammatory drugs from wastewater using 3D-printed device and UHPLC-DAD/FLD analysis 利用3d打印装置和UHPLC-DAD/FLD分析同时提取废水中非甾体类抗炎药

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-09-01 DOI: 10.1016/j.sampre.2025.100210

César Castro-García , Arianna Palermo , Edwin Palacio , Luz O. Leal , Laura Ferrer

Non-steroidal anti-inflammatory drugs (NSAIDs) are widely employed in medicine for their anti-inflammatory and antipyretic properties. Their occurrence has been documented in effluents from wastewater treatment plants (WWTPs), as well as in aquatic ecosystems. NSAIDs are classified as emerging contaminants, thereby underscoring the importance of their environmental monitoring. This study presents a novel approach for the simultaneous on-site extraction of six NSAIDs –acetylsalicylic acid (ASP), celecoxib (CEL), diclofenac (DIC), ibuprofen (IBU), ketoprofen (KET), and naproxen (NAP)– from wastewater, followed by ultra-high performance liquid chromatography coupled with photodiode array and fluorescence detection (UHPLC-DAD/FLD). A 3D-printed device, coated with a highly selective solid-phase extraction (SPE) resin (Oasis HLB®), enabled on-site extraction and preconcentration of the analytes, avoiding to handle large sample volumes. A peristaltic pump helps both retention and elution steps. Method detection limits were 0.12 µg L^-1 for ASP, 0.16 µg L^-1 for CEL and IBU, 1.5 µg L^-1 for DIC, 0.09 µg L^-1 for KET and 0.19 µg L^-1 for NAP. The analytical performance of the 3D-printed device was demonstrated by precision below 5 % and the possibility of reusing up to 24 times without significant loss of extraction efficiency. An AGREEprep score of 0.53 classifies this methodology as moderately green. On-site analysis was conducted at the Calvià WWTP (Mallorca, Spain), where five NSAIDs were detected at various stages, demonstrating the feasibility of the on-site extraction across a broad concentration range. Except for ASP, which exhibited a recovery rate below 47 %, the remaining analytes showed satisfactory recoveries, ranging from 90 to 98 %.

非甾体抗炎药（NSAIDs）因其抗炎和解热的特性而被广泛应用于医学领域。它们在废水处理厂（WWTPs）的流出物以及水生生态系统中都有记录。非甾体抗炎药被归类为新兴污染物，因此强调了其环境监测的重要性。本研究建立了一种从废水中同时现场提取乙酰水杨酸（ASP）、塞来昔布（CEL）、双氯芬酸（DIC）、布洛芬（IBU）、酮洛芬（KET）和萘普生（NAP） 6种非甾体抗炎药的新方法，并采用超高效液相色谱-光电二极管阵列和荧光检测（UHPLC-DAD/FLD）。3d打印设备，涂有高选择性固相萃取（SPE）树脂（Oasis HLB®），可以现场提取和预浓缩分析物，避免处理大样本量。蠕动泵有助于保留和洗脱步骤。方法检出限分别为ASP 0.12µg L-1、CEL和IBU 0.16µg L-1、DIC 1.5µg L-1、KET 0.09µg L-1、NAP 0.19µg L-1。3d打印设备的分析性能被证明精度低于5%，并且可以重复使用多达24次，而不会显著降低提取效率。AGREEprep得分为0.53，将这种方法归类为中度绿色。在calvio污水处理厂（西班牙Mallorca）进行了现场分析，在不同阶段检测到五种非甾体抗炎药，证明了在广泛浓度范围内现场提取的可行性。除ASP回收率低于47%外，其余分析物的回收率均在90% ~ 98%之间，令人满意。

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引用次数: 0

Paper as an ecodesigned and smart material for sample preparation integrated with electrochemical (bio)sensors 纸是一种集成了电化学（生物）传感器的生态设计和智能材料

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-08-20 DOI: 10.1016/j.sampre.2025.100207

Vincenzo Mazzaracchio , Christian Gosti , Laura Belcastro , Fabiana Arduini

Since 2009, paper-based electrochemical biosensors have demonstrated several additional features in analytical chemistry thanks to their capability to manage the fluids by pump-free microfluidics, easily preconcentrate the target analytes, treat the sample with a task-free approach, and detect the target analyte with high sensitivity and accuracy. Herein, we point out the use of paper as a functional material for sample preparation, addressing easily and in a sustainable way the fluid sample management, filtration, separation, centrifugation, chemical sample treatment, and reagent addition. The use of paper for sample preparation in the electrochemical (bio)sensor field is shed light for the first time in a dedicated review. The overriding goal is to highlight the advantages of these cost-effective, environmentally friendly, and easy-to-use devices for smart preparation procedures and accurate electrochemical detection of the target analytes in several fields, including biomedical, environmental, and agrifood.

自2009年以来，基于纸张的电化学生物传感器在分析化学中展示了一些额外的功能，这要归功于它们能够通过无泵微流体管理流体，轻松地预先浓缩目标分析物，以无任务的方法处理样品，并以高灵敏度和准确性检测目标分析物。在此，我们指出使用纸作为一种功能材料来制备样品，以一种容易和可持续的方式解决流体样品管理，过滤，分离，离心，化学样品处理和试剂添加。本文首次介绍了在电化学（生物）传感器领域使用纸张制备样品的情况。最重要的目标是突出这些具有成本效益，环境友好，易于使用的设备的优势，用于智能制备程序和准确的电化学检测目标分析物，包括生物医学，环境和农业食品等多个领域。

引用次数: 0

Advanced solid materials for the extraction of drugs from biological fluids 用于从生物液体中提取药物的先进固体材料

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-08-01 DOI: 10.1016/j.sampre.2025.100202

P. García-Atienza, A. García-Juan, S. Armenta, J.M. Herrero-Martínez, H. Martínez-Pérez-Cejuela

The determination of drugs in biological fluids is essential across various fields, including toxicological analysis, pharmacokinetic studies, and the development of new pharmaceutical products, among others. However, the complexity of biological matrices—due to the presence of endogenous compounds and the typically low concentrations of target analytes—needs efficient sample preparation strategies alongside high-performance instrumentation to achieve the sensitivity and selectivity required in modern analytical chemistry. In response to these challenges, recent advancements have focused on the development of advanced solid materials and their integration with sample preparation techniques. This review highlights recent progress in sorbents with enhanced selectivity, engineered materials such as crystalline frameworks, and the use of biopolymers as natural sorbents for drug analysis in biofluids. Additionally, the application of 3D-printed materials for the fabrication of extraction devices is presented. The article also provides insights into emerging trends and future directions in this evolving field.

生物液体中药物的测定在各个领域都是必不可少的，包括毒理学分析、药代动力学研究和新药品的开发等。然而，生物基质的复杂性——由于内源性化合物的存在和目标分析物的典型低浓度——需要高效的样品制备策略和高性能仪器来实现现代分析化学所需的灵敏度和选择性。为了应对这些挑战，最近的进展集中在先进固体材料的开发及其与样品制备技术的集成上。本文综述了近年来在选择性吸附剂、工程材料（如晶体框架）以及生物聚合物作为天然吸附剂用于生物流体中药物分析方面的进展。此外，还介绍了3d打印材料在提取装置制造中的应用。本文还提供了对这个不断发展的领域的新兴趋势和未来方向的见解。

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引用次数: 0

Greenness of extraction procedures involving biochar-based sorbents for organic compounds 涉及生物炭基吸附剂的有机化合物提取程序的绿色度

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-08-01 DOI: 10.1016/j.sampre.2025.100203

Francesca Merlo, Andrea Speltini, Antonella Profumo

In the field of green sample preparation, new challenges are emerging for guaranteeing sustainability of analytical procedures and remarkable efforts have been made to develop materials from natural and/or renewable sources. In such a scenario, biochar is emerging as alternative sorbent with low economic and environmental impact. It is a carbon-rich material derived from the thermochemical conversion of biomass and waste and endowed with excellent textural properties such as high specific surface area and meso‑ and microporosity, and functional groups that are fundamental for the sorption behaviour, a key point in the analytical performance of biochar. These outstanding properties generated a growing interest in the use of biochar-based sorbents in sample preparation. In this context, this review provides an overview of the last 4-year applications of biochar in extraction techniques through an evaluation of greenness of the sample preparation procedures. At this purpose, two metric tools specific for the sample preparation, as AGREEprep and Sample Preparation Metric of Sustainability (SPMS), have been selected to give comprehensive evaluations about greenness, considering multiple criteria but with different weights and intervals in the parameters. Indeed, the papers here reviewed received in SPMS scores ranging from 5.16 to 10, and in AGREEprep from 0.16 to 0.7, evidencing there is space for improving extraction procedures involving biochar-based sorbents.

在绿色样品制备领域，新的挑战正在出现，以保证分析程序的可持续性和显著的努力已经从自然和/或可再生资源开发材料。在这种情况下，生物炭作为低经济和环境影响的替代吸附剂正在出现。它是一种富含碳的材料，来源于生物质和废物的热化学转化，具有优异的结构特性，如高比表面积、中孔和微孔，以及对吸附行为至关重要的官能团，这是生物炭分析性能的关键点。这些突出的特性引起了人们对在样品制备中使用生物炭基吸附剂的兴趣。在此背景下，本文综述了过去4年生物炭在提取技术中的应用，通过评估样品制备程序的绿色度。为此，选择了两个特定于样品制备的度量工具，即AGREEprep和样品制备可持续性度量（SPMS），考虑多个标准，但在参数中具有不同的权重和间隔，对绿色度进行综合评价。事实上，本文综述的论文在SPMS中的得分在5.16到10之间，在AGREEprep中的得分在0.16到0.7之间，这表明涉及生物炭基吸附剂的提取程序还有改进的空间。

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引用次数: 0

Multiple-shell amorphous Co/Ni-(PO4)x(OH)y hollow layered double hydroxide for enhanced extraction of some azole antifungals from biological samples 多壳无定形Co/Ni-(PO4)x(OH)y空心层状双氢氧化物增强生物样品中某些唑类抗真菌物质的提取

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-08-01 DOI: 10.1016/j.sampre.2025.100209

Maedeh Saadat, Yadollah Yamini

Antifungals drugs are widely used for variety of fungal infections. Extraction and determination of these drugs in biological sample is crucial because of their toxicity, endocrine-disrupting, and cytochrome P450-mediated effects. In addition, developing an efficient and stable sorbent with a high surface area for microextraction by packed sorbent (MEPS) technique is of great interest. Triple-shell Co/Ni-based hydroxide phosphate (TS-CNHP) was synthesized for increasing surface area. For characterization of TS-CNHP, a combination of advanced analytical methods was employed. Field-emission scanning electron microscopy, transmission electron microscopy, Fourier-transform infrared spectroscopy, Brunauer–Emmett–Teller, dynamic light scattering and X-ray diffraction. In this work the MEPS was coupled with high-performance liquid chromatography equipped with an ultraviolet detector (HPLC-UV). The TS-CNHP demonstrated an impressive level of efficiency and the selectivity for the adsorption of azole antifungals. The optimal conditions for MEPS were determined through a systematic evaluation of key parameters influencing analyte extraction efficiency. These parameters included: pH (6), adsorption time (7 min), adsorption cycles (2 cycles), salt addition (0%), elution solvent (methanol), desorption flow rate (100 µL min^-1), desorption volume (400 µL), and desorption cycles (2 cycles). The analytical performance of the method was thoroughly assessed under optimized conditions. The relative standard deviations (RSDs) ranged from 2.7% to 5.4%, demonstrating a high level of precision. Furthermore, extraction recoveries were observed between 78.0% and 89.7%. A wide linear dynamic range (0.5–1000 μg l^-1) and an acceptable LOD (0.2 µg L⁻¹) for all of the analytes were achieved. The coefficients of determination (R²) of ketoconazole, clotrimazole and miconazole are 0.9985, 0.9986 and 0.9989 respectively, which demonstrating the reliability of the method The proposed MEPS-HPLC-UV technique demonstrates remarkable analytical efficiency in the extraction and quantification of trace levels of azole antifungals from biological matrices, specifically dog and human hair.

抗真菌药物广泛用于各种真菌感染。由于这些药物的毒性、内分泌干扰和细胞色素p450介导的作用，在生物样品中提取和测定这些药物至关重要。此外，利用填充吸附剂（MEPS）技术开发一种高效、稳定、高表面积的微萃取吸附剂也具有重要意义。合成了三壳层Co/ ni基氢氧化磷（TS-CNHP），以增加比表面积。为了表征TS-CNHP，结合了先进的分析方法。场发射扫描电子显微镜，透射电子显微镜，傅里叶变换红外光谱，布鲁诺尔-埃米特-泰勒，动态光散射和x射线衍射。在这项工作中，MEPS与配备紫外检测器的高效液相色谱（HPLC-UV）相结合。TS-CNHP表现出了令人印象深刻的效率和选择性吸附唑类抗真菌物质。通过对影响分析物萃取效率的关键参数进行系统评价，确定了MEPS萃取的最佳工艺条件。这些参数包括：pH(6)、吸附时间（7 min）、吸附次数（2次）、加盐量（0%）、洗脱溶剂（甲醇）、解吸流量（100µL min-1）、解吸体积（400µL）、解吸次数（2次）。在优化条件下，对该方法的分析性能进行了全面评价。相对标准偏差（rsd）范围为2.7% ~ 5.4%，具有较高的精度。提取回收率在78.0% ~ 89.7%之间。所有分析物具有宽的线性动态范围（0.5-1000 μg L -1）和可接受的LOD （0.2 μg L -1）。酮康唑、克霉唑和咪康唑的测定系数（R2）分别为0.9985、0.9986和0.9989，证明了该方法的可靠性。MEPS-HPLC-UV技术在提取和定量生物基质（特别是犬和人毛发）中痕量唑类抗真菌药物方面具有良好的分析效率。

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引用次数: 0

Advances in magnetic nanomaterials for biomedical sample pretreatment: synthesis, functionalization, and applications in magnetic solid-phase extraction 生物医学样品前处理用磁性纳米材料的研究进展：合成、功能化及其在磁性固相萃取中的应用

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-08-01 DOI: 10.1016/j.sampre.2025.100208

Jiarui Zhang , Shuang Feng , Yalin Xi , Meiyun Shi , Lei Yin

Magnetic nanomaterials (MNMs) are highly effective sorbents for biomedical sample pretreatment, leveraging their superparamagnetism, large specific surface area, and tunable surface functionalities. This review comprehensively examines MNM classification, synthesis techniques, and functionalization approaches, highlighting their pivotal role in magnetic solid-phase extraction (MSPE) for analyte enrichment. We systematically detail MNM applications in biomedical sample processing, focusing on MSPE for efficient nucleotide isolation, specific protein capture, and ultrasensitive biomarker detection. While MNM-based MSPE offers significant advantages in sensitivity, selectivity, and operational simplicity, challenges remain in achieving reproducible synthesis and deepening the mechanistic understanding of adsorption processes. Future research should prioritize developing automated MSPE platforms and multifunctional MNMs capable of addressing complex clinical matrices. This work provides a valuable reference for designing next-generation analytical systems utilizing MNMs.

磁性纳米材料（MNMs）是生物医学样品预处理的高效吸附剂，利用其超顺磁性、大比表面积和可调表面功能。本文综述了MNM的分类、合成技术和功能化方法，重点介绍了它们在磁固相萃取（MSPE）富集分析物中的关键作用。我们系统地详细介绍了MNM在生物医学样品处理中的应用，重点是MSPE在高效核苷酸分离、特异性蛋白质捕获和超灵敏生物标志物检测方面的应用。虽然基于mnm的MSPE在灵敏度、选择性和操作简单性方面具有显著优势，但在实现可重复性合成和加深对吸附过程机理的理解方面仍然存在挑战。未来的研究应优先开发自动化MSPE平台和能够处理复杂临床基质的多功能MNMs。这项工作为利用纳米微球设计下一代分析系统提供了有价值的参考。

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引用次数: 0

A green approach for electromembrane extraction of morphine from urine using sodium alginate-g-polyacrylic acid/agarose hydrogel membrane 海藻酸钠-聚丙烯酸/琼脂糖水凝胶膜电膜提取尿液中吗啡的绿色方法

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-08-01 DOI: 10.1016/j.sampre.2025.100204

Elnaz Khodabakhshi , Somayeh Makarem , Mehran Kurdtabar , Saeed Nojavan

The development of novel membranes through green chemistry remains a significant challenge in advancing practical separation science. In this study, a sodium alginate-g-polyacrylic acid/agarose hydrogel was synthesized and, for the first time, applied as a membrane in gel electromembrane extraction (G-EME) for the isolation of morphine, a basic analyte, from urine samples. The extracted morphine was subsequently quantified using differential pulse voltammetry (DPV) with a glassy carbon electrode. The hydrogel membrane (5 mm thick) was prepared using 0.75 % (w/v) sodium alginate, 3.80 % (v/v) acrylic acid, 0.04 % (w/v) ammonium persulfate, and 1.25 % (w/v) agarose. The extraction process was optimized by evaluating factors such as membrane composition, extraction time, applied voltage, and pHs of the sample solution, membrane, and acceptor phase (AP). Under optimal conditions (25 min extraction time, 70 V applied voltage, membrane pH 4.0, AP pH 3.0, and sample solution pH 7.0) morphine was efficiently extracted through the hydrogel membrane and transferred to an aqueous AP. The collected AP was mixed with 0.15 M phosphate buffer (pH 7.0) and analyzed voltammetrically. The method achieved a limit of detection of 0.09 μg/mL and a limit of quantification of 0.28 μg/mL, and was successfully applied for morphine determination in urine sample. The polyacrylic acid-based membrane enhanced extraction efficiency through electrostatic interactions, while the use of DPV offered clearer signal interpretation and reduced background current, facilitating reliable detection of trace analytes. These advantages support the method’s potential for simple, selective, and environmentally friendly analysis of basic drugs in biological samples.

通过绿色化学开发新型膜仍然是推进实际分离科学的重大挑战。本研究合成了海藻酸钠-g-聚丙烯酸/琼脂糖水凝胶，并首次应用于凝胶电膜萃取（G-EME）分离尿液中碱性分析物吗啡。随后用玻璃碳电极用差分脉冲伏安法（DPV）对提取的吗啡进行定量。以0.75% （w/v）的海藻酸钠、3.80% （v/v）的丙烯酸、0.04% （w/v）的过硫酸铵和1.25% （w/v）的琼脂糖为原料制备了厚度为5mm的水凝胶膜。通过考察膜组成、提取时间、外加电压、样品溶液ph值、膜和受体相（AP）等因素对提取工艺进行优化。在最佳条件下（提取时间25 min，施加电压70 V，膜pH 4.0, AP pH 3.0，样品溶液pH 7.0），通过水凝胶膜有效提取吗啡，并将其转移到水溶液中。将收集的AP与0.15 M磷酸盐缓冲液（pH 7.0）混合，并进行伏安分析。该方法的检出限为0.09 μg/mL，定量限为0.28 μg/mL，可成功用于尿样中吗啡的检测。聚丙烯酸基膜通过静电相互作用提高了提取效率，而DPV的使用提供了更清晰的信号解释，降低了背景电流，促进了痕量分析物的可靠检测。这些优点支持了该方法对生物样品中基本药物进行简单、选择性和环境友好分析的潜力。

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引用次数: 0