Advances in Sample Preparation最新文献_第4页

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 : 2025-07-07 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 : 2025-07-07 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

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 : 2025-06-30 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

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 : 2025-06-26 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

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 : 2025-06-21 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

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 : 2025-06-04 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

Innovative sample preparation techniques in food analysis: the rise of compressed fluids and novel solvents 食品分析中的创新样品制备技术：压缩流体和新型溶剂的兴起

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-05-23 DOI: 10.1016/j.sampre.2025.100191

Luana C. dos Santos , Juan Felipe Grisales-Mejía , Monique Martins Strieder , Jose A. Mendiola , Elena Ibáñez

Compressed fluids and novel green solvents represent the most promising approaches for achieving sustainable sample preparation in food analysis. Traditional extraction techniques often rely on toxic organic solvents and energy-intensive processes, leading to environmental concerns and inefficient workflows. Green Analytical Chemistry (GAC) promotes the adoption of eco-friendly alternatives that minimize solvent consumption, reduce waste, and enhance extraction efficiency. This review explores the role of compressed fluids’ technologies, including Pressurized Liquid Extraction (PLE), Supercritical Fluid Extraction (SFE), and Gas-Expanded Liquid Extraction (GXL) as viable replacements for conventional solvent-based methods. These techniques offer high selectivity, shorter extraction times, and lower environmental impact. Additionally, novel solvents such as deep eutectic solvents (DES), bio-based alternatives, and gas-expanded liquids present sustainable solutions that improve biodegradability, safety, and solvent recyclability. By integrating these innovative approaches into analytical workflows, food analysis can align with Green Chemistry principles while maintaining high analytical performance. This review critically evaluates the latest advancements in green sample preparation techniques based on pressurized fluids, highlighting their transformative potential in food safety, authenticity verification, and bioactive compound extraction.

压缩流体和新型绿色溶剂代表了在食品分析中实现可持续样品制备的最有前途的方法。传统的提取技术通常依赖于有毒的有机溶剂和能源密集型工艺，导致环境问题和低效的工作流程。绿色分析化学（GAC）提倡采用环保的替代品，最大限度地减少溶剂消耗，减少浪费，提高提取效率。本文综述了压缩流体技术的作用，包括加压液体萃取（PLE）、超临界流体萃取（SFE）和气体膨胀液体萃取（GXL）作为传统溶剂基方法的可行替代品。这些技术具有高选择性、较短的提取时间和较低的环境影响。此外，新型溶剂，如深共晶溶剂（DES）、生物基替代品和气体膨胀液体，提供了可持续的解决方案，提高了生物降解性、安全性和溶剂可回收性。通过将这些创新的方法集成到分析工作流程中，食品分析可以与绿色化学原则保持一致，同时保持高分析性能。这篇综述批判性地评估了基于加压流体的绿色样品制备技术的最新进展，强调了它们在食品安全、真实性验证和生物活性化合物提取方面的变革潜力。

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引用次数: 0

Development of smart samplers and their comparison to dried serum spots for the analysis of growth hormone releasing hormone analogs using LCHRMS/MS LCHRMS/MS分析生长激素释放激素类似物的智能采样器的研制及其与干血清点的比较

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-05-22 DOI: 10.1016/j.sampre.2025.100190

Christina Johannsen , Anna Kha Tu Nguyen , Sasha Shabani , Inger Oulie , Siri Dørum , Yvette Dehnes , Leon Reubsaet , Trine Grønhaug Halvorsen

Growth hormone-releasing hormone (GHRH) analogs, including sermorelin, CJC-1295, and tesamorelin, are prohibited in sports due to their performance-enhancing potential. Detecting these peptides remains challenging, requiring sensitive analytical techniques. This study explores the feasibility of dried serum spots (DSS) and smart samplers for detecting GHRH analogs in human serum using liquid chromatography-high-resolution tandem mass spectrometry. Smart samplers combine sampling and sample preparation in one tool; in this study smart samplers were developed using divinyl sulfone functionalized paper to immobilize antibodies for selective analyte capture. DSS and smart samplers were compared for extraction efficiency, precision, and detection capabilities. Various extraction approaches were evaluated to optimize analyte recovery followed by a blind sample study to assess detection capability at unknown concentrations. Results showed that DSS yielded higher overall signal intensities but exhibited greater variability. In contrast, smart samplers demonstrated improved reproducibility and sensitivity at lower concentrations. Smart samplers successfully identified sermorelin at 0.25 ng∙mL^-1, CJC-1295 at 4 ng∙mL^-1, and tesamorelin at 2.5 ng∙mL^-1, while DSS exhibited limitations at these concentrations. This study presents a proof-of-concept for using smart samplers and DSS in anti-doping analysis. While the results shown are promising, further optimization is needed to improve analyte recovery and sampler stability. The findings support the potential of alternative blood sampling techniques in doping control and peptide biomarker analysis.

生长激素释放激素（GHRH）类似物，包括血清素、CJC-1295和替沙莫瑞林，由于它们具有提高成绩的潜力，被禁止在体育运动中使用。检测这些肽仍然具有挑战性，需要灵敏的分析技术。本研究探讨了使用液相色谱-高分辨率串联质谱法检测人血清中GHRH类似物的干燥血清斑点（DSS）和智能采样器的可行性。智能采样器将采样和样品制备结合在一个工具中；在本研究中，使用二乙烯基砜功能化纸开发了智能采样器，用于固定抗体以进行选择性分析物捕获。比较了DSS和智能采样器的提取效率、精度和检测能力。评估了各种提取方法，以优化分析物回收率，随后进行了盲样研究，以评估未知浓度下的检测能力。结果表明，DSS产生了更高的整体信号强度，但表现出更大的变异性。相比之下，智能采样器在较低浓度下表现出更好的再现性和灵敏度。智能采样器成功地鉴定出0.25 ng∙mL-1的血清素、4 ng∙mL-1的CJC-1295和2.5 ng∙mL-1的替沙莫瑞林，而DSS在这些浓度下表现出局限性。本研究提出了在反兴奋剂分析中使用智能采样器和DSS的概念验证。虽然结果显示很有希望，但需要进一步优化以提高分析物回收率和进样器的稳定性。这些发现支持了替代血液采样技术在兴奋剂控制和肽生物标志物分析中的潜力。

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引用次数: 0

(Natural) deep eutectic solvents in food safety: Innovations in sample preparation 食品安全中的（天然）深共晶溶剂：样品制备的创新

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-05-01 DOI: 10.1016/j.sampre.2025.100188

Laura Carbonell-Rozas, Raquel Capilla-Flores, Roberto Romero-González, Antonia Garrido Frenich

Deep eutectic solvents (DES) and natural deep eutectic solvents (NADES) have emerged as sustainable and efficient alternatives to conventional organic solvents in food safety analysis. These green solvents align with the principles of green analytical chemistry (GAC) by offering biodegradability, low toxicity, and high tunability for different analytical applications. This review critically explores the role of (NA)DES in sample preparation for detecting contaminants in food matrices, highlighting their effectiveness in extracting pesticides, mycotoxins, pharmaceuticals, plastic additives, food additives, and heavy metals. It encompasses diverse sample preparation techniques and food matrices, covering literature published from 2020 to the present. A detailed discussion is provided on the compositions of (NA)DES and their tailor-made capabilities for specific food safety applications. Their integration with advanced extraction techniques such as dispersive liquid-liquid microextraction (DLLME), solid-phase microextraction (SPME), and ultrasound-assisted extraction (UAE) is provided. Additionally, the potential of magnetic and ternary DES is explored, along with other novel DES variants. While the high viscosity of some eutectic mixtures remains a challenge, innovative sample treatment strategies successfully mitigate these limitations, enhancing extraction efficiency and preconcentration capabilities across a wide range of complex food matrices.

深共晶溶剂（DES）和天然深共晶溶剂（NADES）已成为传统有机溶剂的可持续和高效的替代品，用于食品安全分析。这些绿色溶剂符合绿色分析化学（GAC）的原则，为不同的分析应用提供可生物降解性、低毒性和高可调性。本文综述了（NA）DES在检测食品基质中污染物的样品制备中的作用，重点介绍了它们在提取农药、真菌毒素、药物、塑料添加剂、食品添加剂和重金属方面的有效性。它涵盖了多种样品制备技术和食品基质，涵盖了从2020年到现在发表的文献。详细讨论了（NA）DES的组成及其为特定食品安全应用量身定制的能力。它们与先进的萃取技术相结合，如分散液液微萃取（DLLME）、固相微萃取（SPME）和超声辅助萃取（UAE）。此外，探索了磁性和三元DES的潜力，以及其他新型DES变体。虽然一些共晶混合物的高粘度仍然是一个挑战，但创新的样品处理策略成功地缓解了这些限制，提高了在各种复杂食品基质中的提取效率和预富集能力。

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引用次数: 0

Novel gas-diffusion microextraction followed by gas chromatography coupled to tandem mass spectrometry methodology for the determination of fragrance allergens in cosmetic products 新型气相扩散微萃取-气相色谱-串联质谱法测定化妆品中香氛过敏原

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-05-01 DOI: 10.1016/j.sampre.2025.100187

Ana Castiñeira-Landeira , Angel Gomez-Feas , Antonia M. Carro , Thierry Dagnac , Paulo J. Almeida , Maria Llompart

An efficient sample preparation method using gas-diffusion microextraction (GDME) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) is proposed for the first time to determine fragrance allergens in both aqueous and alcohol-based cosmetic products. The most significant GDME parameters were optimized, starting with extraction temperature as a preliminary experiment. Subsequently, an experimental design was performed to evaluate the influence of six parameters: acceptor solution volume, acetonitrile percentage in the acceptor solution, sample dilution, salting-out effect, extraction time, and sample volume. Under the optimized conditions, the method was validated in terms of linearity, precision, trueness, obtaining a good performance. The validated methodology was applied to twelve real cosmetic samples, demonstrating the widespread occurrence of these allergens in cosmetics. Notably, lilial, a compound prohibited by Regulation EC No 1223/2009, was detected in one cosmetic product (460 μg mL^-1); and the concentrations of some of the target fragrance allergens in some samples reach values above 1000 μg mL^-1. This methodology represents a sustainable and practical approach, supported by AGREEPrep and BAGI metrics, respectively.

首次建立了气相扩散微萃取(GDME) -气相色谱-串联质谱（GC-MS/MS）联用的高效样品制备方法，用于测定水基和醇基化妆品中的香氛过敏原。从提取温度作为初步实验入手，优化了最显著的GDME参数。随后，进行了实验设计，以评估六个参数的影响：受体溶液体积、受体溶液中乙腈的百分比、样品稀释度、盐析效果、提取时间和样品体积。在优化条件下，对该方法进行了线性度、精密度、准确度等方面的验证，取得了较好的效果。经验证的方法应用于12个真实化妆品样品，表明这些过敏原在化妆品中广泛存在。值得注意的是，在一种化妆品中检测到460 μg mL-1的丁香，这是欧盟法规1223/2009禁止的化合物；部分样品中目标香氛过敏原的浓度达到1000 μg mL-1以上。该方法代表了一种可持续和实用的方法，分别得到AGREEPrep和BAGI指标的支持。

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引用次数: 0