Advances in Sample Preparation最新文献_第4页

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 Epub Date: 2025-08-30 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

Pretreat immunosuppressants in whole blood without vortexing and centrifugation 在全血中预处理免疫抑制剂，不进行旋流和离心

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-08-01 Epub Date: 2025-07-07 DOI: 10.1016/j.sampre.2025.100198

Rui Zhang , Ren-Jie Yang , Ping-An Zhang , Shao-Ting Wang

Background

Precise measurement of immunosuppressant levels in whole blood is critical for monitoring post-transplant patient outcomes. Conventional protein precipitation (PP) methods, which rely on vortex mixing and centrifugation, present substantial limitations in terms of automation and scalability. To address these challenges, we developed a novel pretreatment strategy termed “Pseudo-Protein-Precipitation combined with Cold-Induced Phase Separation” (PPP+CIPS), designed to simplify sample processing and enhance high-throughput efficiency.

Results

The PPP+CIPS method employs 48 % acetonitrile to generate a semi-homogeneous blood suspension, enabling in-situ drug extraction via CIPS. Notably, this approach eliminates the need for vortexing and centrifugation—key bottlenecks in traditional therapeutic drug monitoring workflows. By leveraging 96-well plates and multi-channel pipettes, the protocol reduces pretreatment time to approximately one-third of that required by PP. Clinical validation (n = 288 in total) revealed strong concordance with established methods, with 94 % of tacrolimus, 95 % of cyclosporin A, and 92 % of sirolimus measurements falling within ±20 % agreement limits.

Significance

The PPP+CIPS strategy marks a significant leap forward in high-throughput therapeutic drug monitoring for immunosuppressants. Its seamless integration with 96-well formats and static processing workflows makes it a promising cornerstone for future automated and integrated TDM systems.

背景：精确测量全血免疫抑制剂水平对于监测移植后患者的预后至关重要。传统的蛋白质沉淀（PP）方法依赖于涡旋混合和离心，在自动化和可扩展性方面存在很大的局限性。为了应对这些挑战，我们开发了一种新的预处理策略，称为“伪蛋白质沉淀结合冷诱导相分离”（PPP+CIPS），旨在简化样品处理并提高高通量效率。结果PPP+CIPS方法采用48%乙腈制备半均质血悬液，可通过CIPS进行原位药物提取。值得注意的是，这种方法消除了传统治疗药物监测工作流程中的关键瓶颈——涡流和离心的需要。通过利用96孔板和多通道移液器，该方案将预处理时间减少到PP所需时间的约三分之一。临床验证（总共288例）显示与既定方法具有很强的一致性，94%的他克莫司，95%的环孢素A和92%的西罗莫司测量值在±20%的一致性范围内。PPP+CIPS策略标志着免疫抑制剂高通量治疗药物监测的重大飞跃。它与96井格式和静态处理工作流程的无缝集成使其成为未来自动化和集成TDM系统的基石。

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引用次数: 0

Supported liquid membrane-coupled Extraction 支撑液膜耦合萃取

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-08-01 Epub Date: 2025-07-07 DOI: 10.1016/j.sampre.2025.100197

Shengjie Hu , Xiantao Shen , Chuixiu Huang

Group separation of multiple analytes with diverse physicochemical properties from the same complex sample is significant in clinical diagnosis, environmental monitoring and biomarker identification. To achieve this goal, supported liquid membrane (SLM)-coupled extraction techniques were developed by integrating two or more SLM-based extraction processes, either simultaneously or sequentially. This approach offers several advantages such as low sample consumption, short operational time, and efficient group separation. In recent years, SLM-coupled extraction approaches have been successfully applied to extract multiple targets from complex biological samples and environmental samples. However, the reviews in the literature mainly focused on a single SLM extraction technique, either liquid-phase microextraction (LPME) or electromembrane extraction (EME). Therefore, a comprehensive overview of SLM-coupled extraction techniques is still lack. The current review comprehensively summarizes the advances in SLM-coupled extraction techniques. We elaborate three types of SLM-coupled extraction techniques, including coupled-LPME, coupled-EME and EME/LPME. Moreover, a prospective discussion on the future development trends of the SLM-coupled extraction techniques is also provided.

从同一复杂样品中分离具有不同理化性质的多种分析物在临床诊断、环境监测和生物标志物鉴定中具有重要意义。为了实现这一目标，支持液膜（SLM）耦合萃取技术通过同时或顺序整合两个或多个基于SLM的萃取过程而开发出来。该方法具有样品消耗少、操作时间短、组分离效率高等优点。近年来，slm耦合提取方法已成功应用于从复杂生物样品和环境样品中提取多靶点。然而，文献综述主要集中在单一的SLM提取技术，即液相微萃取（LPME）或电膜萃取（EME）。因此，对slm耦合提取技术的全面概述仍然缺乏。本文综述了slm耦合萃取技术的研究进展。我们详细介绍了三种类型的slm耦合提取技术，包括耦合-LPME、耦合-EME和EME/LPME。并对slm耦合萃取技术的未来发展趋势进行了展望。

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引用次数: 0

Green solvents and enzymes combined with advanced extraction techniques for the recovery of bioactive carotenoids and extractable/non-extractable polyphenols from grapefruit peels 绿色溶剂和酶结合先进的提取技术，从葡萄柚皮中回收生物活性类胡萝卜素和可提取/不可提取的多酚

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-08-01 Epub Date: 2025-06-04 DOI: 10.1016/j.sampre.2025.100192

Gloria Domínguez-Rodríguez , María Concepción García , María Luisa Marina

The simultaneous extraction of extractable phenolic compounds (EPPs) and carotenoids from grapefruit peels using microwave-assisted extraction (MAE) with biobased solvents was optimized, followed by non-extractable polyphenols (NEPs) extraction. Ethyl acetate:γ-valerolactone (20:80 v/v) yielded the highest antioxidant and anti-inflammatory EPPs at 50 °C in 6 min. From the residue, NEPs were obtained by comparing several methods: ultrasound-assisted extraction (UAE) combined with enzymatic-assisted extraction (EAE), and UAE and MAE with natural deep eutectic solvents (NaDES). UAE (15 min, 30 % amplitude) followed by EAE (70 °C, 40 min) and MAE-NaDES using choline chloride:lactic acid (1:2, 50 % water, 50 °C, 6 min) yielded the most bioactive NEPs. HPLC-DAD-QTOF-MS analysis allowed to identified 19 polyphenols in both extracts, highlighting naringin as the majority, particularly in UAE-EAE extract. Stability tests showed UAE-EAE extracts protect against oxidative damage, potentially extending the shelf life of food products. On the other hand, MAE-NaDES extracts prevent anti-inflammatory compound degradation, indicating their potential application in pharmaceutical formulations. Thus, depending on the purpose, either UAE-EAE or MAE-NaDES can be used.

优化了生物基溶剂微波辅助提取法（MAE）同时提取葡萄柚皮中可提取酚类化合物（EPPs）和类胡萝卜素，其次是不可提取多酚类物质（NEPs）。乙酸乙酯：γ-戊内酯（20:80 v/v）在50°C、6 min条件下得到的抗氧化和抗炎epp最高。通过超声辅助提取（UAE）和酶辅助提取（EAE）、UAE和MAE与天然深共晶溶剂（NaDES）的比较得到NEPs。阿联酋（15分钟，30%振幅），其次是EAE（70°C， 40分钟）和使用氯化胆碱：乳酸（1:2,50%水，50°C， 6分钟）的MAE-NaDES产生了最具生物活性的NEPs。HPLC-DAD-QTOF-MS分析发现，两种提取物中均含有19种多酚，其中柚皮苷含量最高，在UAE-EAE提取物中含量最高。稳定性测试表明，阿联酋- eae提取物可以防止氧化损伤，可能延长食品的保质期。另一方面，MAE-NaDES提取物可防止抗炎化合物降解，表明其在药物制剂中的潜在应用。因此，根据不同的目的，可以使用UAE-EAE或MAE-NaDES。

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引用次数: 0

Enhanced electromembrane extraction of acidic drugs using a chitosan-agarose hybrid gel membrane 壳聚糖-琼脂糖混合凝胶膜对酸性药物电膜萃取的强化作用

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-08-01 Epub Date: 2025-06-30 DOI: 10.1016/j.sampre.2025.100196

Hasti Gharah Sheikhlou , Majid Gharah Sheikhlou , Marzieh Saberi , Saeed Nojavan

In this study, a novel chitosan-agarose gel membrane was developed and applied in the gel electromembrane extraction (G-EME) technique to extract and preconcentrate two model acidic drugs, naproxen and ibuprofen, from urine samples. Chitosan, acting as a positively charged agent and viscosifier, significantly improved extraction efficiency by reducing electric current and minimizing the electroendosmosis (EEO) effect. The parameters affecting the extraction recoveries were optimized and evaluated using both one-variable-at-a-time and Box–Behnken design approaches alongside response surface methodology. To maximize drugs recovery from a 7.0 mL urine sample, the following parameters were optimized: a membrane composed of 3.0 % (w/v) agarose and 1.0 % (w/v) chitosan, pH of the gel membrane: 5.5, extraction voltage: 32.5 V, pH of the donor phase: 8.0, pH of the acceptor phase: 11.0, extraction time: 21 min, volume of acceptor phase: 200 µL, gel membrane thickness: ∼ 4 mm and donor phase stirring speed: 500 rpm. Under optimal conditions, the extraction recoveries were 60.4 % for naproxen and 81.9 % for ibuprofen. Limits of detection for naproxen and ibuprofen were 3.0 and 4.5 ng/mL, respectively. This method was successfully applied to quantify acidic drugs in real urine samples, achieving relative recoveries in the range of 91.2–94.9 %, demonstrating excellent reliability for biological matrices.

本研究开发了一种新型壳聚糖-琼脂糖凝胶膜，并将其应用于凝胶电膜萃取（G-EME）技术中，用于从尿液样品中提取和预浓缩两种模型酸性药物萘普生和布洛芬。壳聚糖作为一种带正电荷的助剂和增粘剂，通过减小电流和降低EEO效应，显著提高了提取效率。采用单变量法和Box-Behnken设计方法以及响应面法对影响提取回收率的参数进行了优化和评价。为了最大限度地从7.0 mL尿液样品中回收药物，优化了以下参数：凝胶膜由3.0% （w/v）琼脂糖和1.0% （w/v）壳聚糖组成，凝胶膜pH: 5.5，提取电压：32.5 v，给体相pH: 8.0，受体相pH: 11.0，提取时间：21 min，受体相体积：200µL，凝胶膜厚度：~ 4 mm，给体相搅拌速度：500 rpm。在最佳提取条件下，萘普生的提取率为60.4%，布洛芬的提取率为81.9%。萘普生和布洛芬的检出限分别为3.0和4.5 ng/mL。该方法成功地应用于实际尿液样品中酸性药物的定量，相对回收率为91.2 ~ 94.9%，对生物基质具有良好的可靠性。

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引用次数: 0

Recent green approaches in liquid-phase microextraction 液相微萃取的绿色新方法

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-08-01 Epub Date: 2025-07-17 DOI: 10.1016/j.sampre.2025.100201

Miguel Ángel Aguirre , Natalia Arroyo-Manzanares , Laura Carbonell-Rozas , José Grau , Carlos Moreno , Lorena Vidal

The miniaturization of conventional extraction techniques, particularly microextraction methods, has led to a reduction in the use of hazardous reagents and waste. However, the continued use of toxic solvents and materials, along with time-consuming sample preparation processes, negatively impacts the overall sustainability of these methods. As a result, there is growing interest in exploring greener alternatives. This review highlights the most promising green solvents for liquid-phase microextraction, including (natural) deep eutectic solvents, low-toxicity ionic liquids, surfactants, micellar solvents, and bio-based solvents, emphasizing their applications in innovative sample preparation techniques in the last five years. Particular emphasis is placed on their use in automated and semi-automated systems, in line with the increasing role of automation in Analytical Chemistry. Selected applications have been carefully reviewed and discussed to illustrate key advances in the use of green solvents and automation for extracting a wide range of compounds from various matrices. In addition, future perspectives are outlined to guide further development of liquid-phase microextraction in alignment with current trends in green sample preparation.

传统萃取技术，特别是微萃取方法的小型化，减少了危险试剂和废物的使用。然而，有毒溶剂和材料的持续使用，以及耗时的样品制备过程，对这些方法的整体可持续性产生了负面影响。因此，人们对探索更环保的替代品越来越感兴趣。本文综述了液相微萃取中最有前途的绿色溶剂，包括（天然）深共晶溶剂、低毒离子液体、表面活性剂、胶束溶剂和生物基溶剂，并重点介绍了近五年来它们在创新样品制备技术中的应用。特别强调的是它们在自动化和半自动化系统中的使用，以配合自动化在分析化学中日益重要的作用。选定的应用程序已经仔细审查和讨论，以说明使用绿色溶剂和自动化从各种基质中提取广泛的化合物的关键进展。此外，概述了未来的前景，以指导液相微萃取的进一步发展，以符合当前绿色样品制备的趋势。

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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 Epub Date: 2025-07-29 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

Improved sample preparation using bead mill homogenization 改进了球磨均质法制备样品的方法

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-08-01 Epub Date: 2025-06-21 DOI: 10.1016/j.sampre.2025.100194

Madison E. Walbrun , Aamna Aijaz , Gabriella Ryan , John D. Bunting , Zachary P. Morehouse , Rodney J. Nash

Proper sample preparation is the key to having successful data analysis downstream. Despite the many efforts to improve sample preparation, there are still many inconsistencies and challenges when attempting to produce a sample for downstream analysis. Here we compare common methods used in sample preparation (detergent and manual Dounce homogenization) to mechanical Bead Mill homogenization. These methods have been shown to lyse both cell and tissue, however, concentrations and detectability of desired analytes can be greatly reduced. These results show that mechanical Bead Mill homogenization requires less starting sample, and less time, while producing higher protein concentrations with increased reproducibility, therefore improving downstream analysis.

正确的样品制备是下游数据分析成功的关键。尽管在改进样品制备方面做出了许多努力，但在试图生产用于下游分析的样品时，仍然存在许多不一致和挑战。在这里，我们比较了样品制备中常用的方法（洗涤剂和手动Dounce均质）和机械珠磨均质。这些方法已被证明可以裂解细胞和组织，然而，所需分析物的浓度和可检测性会大大降低。这些结果表明，机械球磨均质需要更少的起始样品和更少的时间，同时产生更高的蛋白质浓度，增加了再现性，从而改善了下游分析。

引用次数: 0

Evaluation of performance and matrix compatibility of mixed mode C18-SCX SPME fibers for compounds with different physicochemical properties 混合模式C18-SCX SPME纤维对不同理化性质化合物的性能及基质相容性评价

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-08-01 Epub Date: 2025-06-26 DOI: 10.1016/j.sampre.2025.100195

Marcos Tascon , Ezel Boyaci , Nathaly Reyes-Garcés , Janusz Pawliszyn

Solid-phase microextraction (SPME) has evolved significantly since its inception, yet challenges remain in developing coatings fully compatible with LC-MS that combine broad polarity coverage with biocompatibility for complex matrices. This study evaluates mixed-mode C₁₈-SCX (strong cation exchange) SPME fibers designed to extract analytes of a wide range of physicochemical properties, addressing limitations in current methodologies. The fibers were tested for extraction efficiency, reproducibility, and matrix compatibility using a group of model compounds with different physicochemical properties, namely, codeine (logP=1.19), carbamazepine (logP=2.45), diazepam (logP=2.82), and propranolol (logP=3.47). Furthermore, the biocompatibility was tested in diverse matrices, such as PBS, blood, plasma, urine, and grape juice.

Results demonstrated exceptional inter-fiber reproducibility (RSD ≤ 15 %, n = 96 fibers) and robust performance in biomatrices, with relative matrix effects primarily governed by analyte binding affinities to matrix macromolecules rather than coating fouling. Absolute matrix effects were negligible (93–111 %), underscoring the fibers’ ability to deliver clean extracts for LC-MS analysis. Fiber reusability was validated over three consecutive extractions (RSD ≤ 10 %), and morphological integrity was preserved post-extraction, even in challenging matrices like whole blood. This work represents the versatility of mixed-mode SPME fibers for high-throughput bioanalysis, offering a significant advancement for in vivo and in vitro targeted and untargeted applications.

固相微萃取（SPME）技术自问世以来发展迅速，但在开发与LC-MS完全兼容的涂层方面仍然存在挑战，这种涂层结合了广泛的极性覆盖和复杂基质的生物相容性。本研究评估了混合模式C18-SCX（强阳离子交换）SPME纤维，该纤维设计用于提取各种物理化学性质的分析物，解决了当前方法的局限性。使用一组物理化学性质不同的模型化合物，即可待因（logP=1.19）、卡马西平（logP=2.45）、地西泮（logP=2.82）和心得安（logP=3.47），对纤维的提取效率、重现性和基质相容性进行了测试。此外，生物相容性测试在不同的基质，如PBS，血液，血浆，尿液和葡萄汁。结果表明，该材料具有优异的纤维间重现性（RSD≤15%,n = 96根纤维），在生物基质中具有强大的性能，其相对基质效应主要由分析物与基质大分子的结合亲和力而不是涂层污染决定。绝对基质效应可以忽略不计（93 - 111%），强调纤维提供清洁提取物用于LC-MS分析的能力。在连续三次提取中验证了纤维的可重用性（RSD≤10%），并且即使在全血等具有挑战性的基质中，提取后也保持了形态完整性。这项工作代表了混合模式SPME纤维在高通量生物分析中的多功能性，为体内和体外靶向和非靶向应用提供了重大进展。

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引用次数: 0

A 3D-printed handheld device for quick citrus tissue lysis and nucleic acid extraction 用于快速柑橘组织裂解和核酸提取的3d打印手持设备

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-08-01 Epub Date: 2025-07-10 DOI: 10.1016/j.sampre.2025.100199

Chia-Wei Liu , Brent Kalish , Sohrab Bodaghi , Georgios Vidalakis , Hideaki Tsutsui

A 3D-printed handheld device has been developed for rapid and efficient sample preparation, extracting pathogen total nucleic acids from citrus leaves for downstream molecular analysis. With its high-speed motor, knurled lysis chamber for rapid sample lysis, and quick nucleic acid extraction using cellulose paper disks (Whatman CHR1), this device can yield ready-to-use DNA and RNA in just 12 min. All components, except for the motor, wiring, and paper disks, were printed in-house using a PolyJet 3D printer with photosensitive resins. The device was optimized for maximum sample lysis by evaluating operation voltages and chamber features, as measured by DNA and RNA concentrations using a Qubit fluorometer and quantification cycle (Cq) values obtained through qPCR assays. The results showed that the lysis chamber with internal knurling and the motor operated at 7.5 V was sufficient for effective sample lysis in 1 min, achieving RNA concentrations up to 87.6 % of those obtained with mortar-and-pestle grinding. Paper disk washing and elution conditions were also optimized using a NanoDrop spectrophotometer and qPCR assays, where two 1-minute washes and a 100 µL elution volume resulted in the highest purity and lowest Cq value. The optimized handheld device was validated with citrus sources infected with Citrus tristeza virus (CTV) and Spiroplasma citri (S. citri), demonstrating high detection accuracy (100 %) and low assay variation (CV < 3.8 %) in qPCR-based analysis. Based on these successful results, this device is expected to be broadly applicable to similar viral and bacterial pathogens affecting plants.

开发了一种3d打印手持设备，用于快速高效的样品制备，从柑橘叶片中提取病原体总核酸，用于下游分子分析。凭借其高速电机，用于快速样品裂解的滚花裂解室，以及使用纤维素纸盘（Whatman CHR1）的快速核酸提取，该设备可以在12分钟内产生即用型DNA和RNA。除了电机，线路和纸盘外，所有组件都使用PolyJet带有光敏树脂的3D打印机进行内部打印。通过评估操作电压和腔室特征，通过使用量子比特荧光仪测量DNA和RNA浓度以及通过qPCR分析获得的定量周期（Cq）值，对该装置进行了优化，以实现最大的样品裂解。结果表明，内置滚花的裂解室和在7.5 V下工作的马达足以在1 min内有效裂解样品，其RNA浓度达到杵臼研磨的87.6%。利用NanoDrop分光光度计和qPCR对纸盘洗涤和洗脱条件进行了优化，其中两次1分钟洗涤和100µL洗脱量可获得最高纯度和最低Cq值。优化后的手持设备在柑橘源感染柑橘tristeza病毒（CTV）和柑橘螺旋体（S. citri）的柑橘源中进行了验证，显示出较高的检测准确率（100%）和较低的检测变异(CV <；3.8%)。基于这些成功的结果，该装置有望广泛应用于影响植物的类似病毒和细菌病原体。

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