Advances in Sample Preparation最新文献

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Nasal exudate sampling for GFAP determination: A comparative study of collection devices and recovery methods for point-of-care stroke diagnosis 鼻渗出液取样测定GFAP:收集装置和恢复方法在护理点脑卒中诊断中的比较研究
IF 6.6
Advances in Sample Preparation Pub Date : 2026-10-01 Epub Date: 2026-10-06 DOI: 10.1016/j.sampre.2026.100249
Pablo Rioboó-Legaspi, Estefanía Costa-Rama, Beatriz Fernández, Carmen García-Cabo, Lorena Fernández-Benavente, Sergio Calleja-Puerta, M. Teresa Fernández-Abedul
{"title":"Nasal exudate sampling for GFAP determination: A comparative study of collection devices and recovery methods for point-of-care stroke diagnosis","authors":"Pablo Rioboó-Legaspi,&nbsp;Estefanía Costa-Rama,&nbsp;Beatriz Fernández,&nbsp;Carmen García-Cabo,&nbsp;Lorena Fernández-Benavente,&nbsp;Sergio Calleja-Puerta,&nbsp;M. Teresa Fernández-Abedul","doi":"10.1016/j.sampre.2026.100249","DOIUrl":"10.1016/j.sampre.2026.100249","url":null,"abstract":"<div><div>The discovery of a brain-nose discharge through the glymphatic clearance pathway across the cribriform plate has opened new possibilities for biomarker-based diagnostics of neurological disorders. Glial fibrillary acidic protein (GFAP) is a clinically relevant biomarker for early differentiation between hemorrhagic and ischemic stroke, yet its low abundance in nasal exudate (NE) poses significant analytical challenges. Current nasal sampling devices and processing workflows are commonly aimed at infectious respiratory diseases, where analyte concentrations are substantially higher. In this study, three NE collection devices (flocked nylon swabs, GrooveSwab<sup>Ⓡ</sup>, and Nasosorption™ swabs) have been evaluated alongside multiple recovery protocols for their effectiveness in recovering GFAP from NE. Flocked nylon swabs demonstrated superior protein recovery and patient comfort, making them the most appropriate option for GFAP determination. In contrast, although GrooveSwab<sup>Ⓡ</sup> and Nasosorption™ swabs exhibited lower protein recovery, they showed potential for applications involving higher analyte concentrations or alternative diagnostic formats. Recovery protocols combining vortexing and centrifugation provided the highest GFAP release with minimal losses. Overall, these findings support the feasibility of decentralized NE sampling for GFAP determination and highlight its potential integration into rapid, minimally invasive point-of-care workflows for stroke diagnosis.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"20 ","pages":"Article 100249"},"PeriodicalIF":6.6,"publicationDate":"2026-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149156869","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Natural deep eutectic solvents for sustainable bioactive compound extraction: Fundamentals, emerging technologies, current scale-up challenges, and future industrial perspectives 用于可持续生物活性化合物提取的天然深层共晶溶剂:基本原理、新兴技术、当前规模挑战和未来工业前景
IF 6.6
Advances in Sample Preparation Pub Date : 2026-10-01 Epub Date: 2026-09-27 DOI: 10.1016/j.sampre.2026.100248
Hla Myo, Desy Liana, Anuchit Phanumartwiwath
{"title":"Natural deep eutectic solvents for sustainable bioactive compound extraction: Fundamentals, emerging technologies, current scale-up challenges, and future industrial perspectives","authors":"Hla Myo,&nbsp;Desy Liana,&nbsp;Anuchit Phanumartwiwath","doi":"10.1016/j.sampre.2026.100248","DOIUrl":"10.1016/j.sampre.2026.100248","url":null,"abstract":"<div><div>The global transition toward sustainable manufacturing has intensified interest in eco-friendly solvent systems for extracting bioactive compounds from natural matrices. Conventional petroleum-derived solvents, such as hexane, methanol, and acetone, remain efficient but increasingly criticized for their volatility, toxicity, and poor biodegradability, all of which contravene the principles of green chemistry and circular bioeconomy. Over the past decade, alternative solvent classes including ionic liquids (ILs), deep eutectic solvents (DESs) and their natural analogues- natural deep eutectic solvents (NADESs), supercritical fluids (SCFs), and hybrid co-solvent systems have emerged as promising substitutes. As aforementioned, NADESs have attracted particular attention for their renewable origin, molecular tunability, low volatility, and capacity to dissolve structurally diverse phytochemicals such as polyphenols, flavonoids, alkaloids, carotenoids, and essential oils. Despite these advances, significant barriers still impede industrial adoption. The high viscosity and mass-transfer resistance of NADES, limited recyclability, incomplete toxicological profiling, and lack of standardized metrics for solvent “greenness” continue to challenge scalability. Moreover, techno-economic feasibility, process integration, and regulatory acceptance remain insufficiently investigated at the pilot and commercial levels. This review provides a comprehensive and critical evaluation of recent progress in NADES-based extraction of bioactive compounds, focusing on their physicochemical properties, molecular interaction mechanisms, extraction kinetics, and environmental performance. Key challenges related to process optimization, solvent recovery, life-cycle assessment, and safety evaluation are discussed. Finally, strategic perspectives are proposed to guide the development of next-generation natural eutectic solvent systems that are not only efficient and selective but also safe, economically viable, and aligned with sustainable industrial practices.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"20 ","pages":"Article 100248"},"PeriodicalIF":6.6,"publicationDate":"2026-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149156871","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Microsolid-phase extraction (µSPEed) for crizotinib preconcentration prior to rapid chiral analysis by electrokinetic chromatography 微固相萃取(µSPEed)在电动色谱快速手性分析之前进行克唑替尼预浓缩
IF 6.6
Advances in Sample Preparation Pub Date : 2026-10-01 Epub Date: 2026-10-12 DOI: 10.1016/j.sampre.2026.100252
Laura García-Cansino, María Ángeles García, María Luisa Marina
{"title":"Microsolid-phase extraction (µSPEed) for crizotinib preconcentration prior to rapid chiral analysis by electrokinetic chromatography","authors":"Laura García-Cansino,&nbsp;María Ángeles García,&nbsp;María Luisa Marina","doi":"10.1016/j.sampre.2026.100252","DOIUrl":"10.1016/j.sampre.2026.100252","url":null,"abstract":"<div><div>The impact of chirality in pharmaceutical and environmental fields requires the development of sensitive stereoselective methodologies for pharmaceutical quality control and drug determination in environmental samples. An ultrafast enantioselective electrokinetic chromatography (EKC) method was developed for the chiral analysis of the anticancer drug crizotinib. The enantiomeric separation was achieved within 2.9 min with a resolution of 3.3 using 4 mM sulfated-γ-cyclodextrin in 25 mM formate buffer (pH 3.0). S-crizotinib, the enantiomeric impurity, migrated before the active R-enantiomer avoiding peaks overlapping facilitating its detection in enantiopure pharmaceutical formulations. The analytical performance was evaluated in terms of linearity, selectivity, trueness, precision, and sensitivity. Excellent linearity (R<sup>2</sup> &gt; 0.999), precision with RSD values below 5.3% for corrected peak areas, and recoveries of 101-103% were established. Limits of detection (LODs) were 0.2 and 0.3 mg L<sup>−1</sup> for S- and R-enantiomers, respectively, enabling the detection of S-crizotinib at the 0.1% level relative to R-crizotinib, as established by ICH regulations. The analysis of a commercial pharmaceutical formulation confirmed the labeled R-crizotinib content (100-101%), with no detectable enantiomeric impurity. For wastewater analysis, microsolid-phase extraction (µSPEed) was optimized to improve method sensitivity providing a 15-fold enrichment, recoveries of 93-101%, and LODs of 13 and 20 µg L<sup>−1</sup> for S- and R-crizotinib, respectively. Greenness assessment of the µSPEed-EKC strategy using complementary metrics showed a favorable environmental profile, with Eco-Scale, AGREE, ComplexGAPI, and BAGI scores of 89, 0.70, 78, and 60, respectively. The developed methodology represents a rapid, sustainable and sensitive analytical tool for crizotinib determination at µg L<sup>−1</sup> levels.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"20 ","pages":"Article 100252"},"PeriodicalIF":6.6,"publicationDate":"2026-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149212368","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A supramolecular solvent approach for internal exposome characterization in human serum: An exploratory proof-of-concept study in patients with serious mental illness 一种用于人血清内部暴露表征的超分子溶剂方法:一项针对严重精神疾病患者的探索性概念验证研究
IF 6.6
Advances in Sample Preparation Pub Date : 2026-10-01 Epub Date: 2026-09-27 DOI: 10.1016/j.sampre.2026.100250
Cristina de Dios Pérez, Ana Ballesteros-Gómez, María José Jaén Moreno, Fernando Sarramea Crespo, Soledad Rubio
{"title":"A supramolecular solvent approach for internal exposome characterization in human serum: An exploratory proof-of-concept study in patients with serious mental illness","authors":"Cristina de Dios Pérez,&nbsp;Ana Ballesteros-Gómez,&nbsp;María José Jaén Moreno,&nbsp;Fernando Sarramea Crespo,&nbsp;Soledad Rubio","doi":"10.1016/j.sampre.2026.100250","DOIUrl":"10.1016/j.sampre.2026.100250","url":null,"abstract":"<div><div>Straightforward analytical strategies for exploring the chemical exposome in serum can provide a valuable framework for characterizing exposure patterns across different populations. With this aim, we present a supramolecular solvent (SUPRAS)-based microextraction method coupled with liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) for multiclass xenobiotic analysis in human serum. Quantitative analysis and different screening workflows were combined to maximize coverage of the detectable chemical space. The method integrates tetrahydrofuran (THF)-assisted protein precipitation with 1-hexanol-driven SUPRAS formation and extraction into a single step, enabling efficient recovery of chemically diverse compounds (log D<sub>7.4</sub> − 1.7 to 7) while minimizing solvent consumption (400 µL per sample) and simplifying sample handling to a straightforward mixing and centrifugation procedure. After optimization of SUPRAS composition and serum volume, absolute extraction efficiencies of 70–120% were achieved for most analytes, with controlled matrix effects and no additional clean-up. The potential applicability of the developed workflow to real clinical samples was explored through a proof-of-concept study involving individuals with serious mental illness (SMI).</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"20 ","pages":"Article 100250"},"PeriodicalIF":6.6,"publicationDate":"2026-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149156870","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Electromembrane extraction of basic pharmaceuticals from biological matrices using a micro-pillar stabilized liquid membrane 微柱稳定液膜电膜萃取生物基质中基本药物
IF 6.6
Advances in Sample Preparation Pub Date : 2026-10-01 Epub Date: 2026-10-06 DOI: 10.1016/j.sampre.2026.100251
Anna Thu Hoai Nguyen, Nickolaj J. Petersen, Steven Ray Haakon Wilson, Frøydis Sved Skottvoll, Frederik Andre Hansen, Stig Pedersen-Bjergaard, Jörg P. Kutter
{"title":"Electromembrane extraction of basic pharmaceuticals from biological matrices using a micro-pillar stabilized liquid membrane","authors":"Anna Thu Hoai Nguyen,&nbsp;Nickolaj J. Petersen,&nbsp;Steven Ray Haakon Wilson,&nbsp;Frøydis Sved Skottvoll,&nbsp;Frederik Andre Hansen,&nbsp;Stig Pedersen-Bjergaard,&nbsp;Jörg P. Kutter","doi":"10.1016/j.sampre.2026.100251","DOIUrl":"10.1016/j.sampre.2026.100251","url":null,"abstract":"<div><div>In this work, a reusable microfluidic device for electromembrane extraction (EME) was fabricated from stoichiometric thiol-ene and evaluated for the extraction of a large set of pharmaceuticals across a broad polarity range and from urine and saliva samples. The device featured micro-pillar arrays for stabilization and straightforward renewal of the liquid membrane, enabling repeated use of the same microchip. The thiol-ene material provided a suitable balance of hydrophobic and hydrophilic properties, allowing controlled handling of both aqueous solutions and organic liquid membranes.</div><div>Extractions were performed at sample and acceptor flow rates of 2.0 µL/min, an extraction potential of 2.0 V, and an extraction time of 10 minutes, using liquid membranes of different polarity. In total, the system was evaluated for the extraction of 61 basic pharmaceuticals covering log P values from -0.5 to 5.0 in water, urine, and saliva. Depending on membrane and matrix composition, typical recoveries were around 40%, while stable operation was observed with all three matrices.</div><div>The method showed favorable greenness, with low power consumption and minimal waste generation. The thiol-ene microchip has a mass of 16 g and was reused for multiple extractions, while only 0.1 µL of liquid membrane was discarded per extraction, corresponding to more than 99.9% material reuse. Overall, this system provided a sustainable, reusable, and versatile microfluidic platform for EME of pharmaceuticals from biological fluids.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"20 ","pages":"Article 100251"},"PeriodicalIF":6.6,"publicationDate":"2026-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149156868","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Corrigendum to “From colloids to dendrites: Silica nanoparticles as advanced solid-phase extraction sorbents for sample preparation in the analysis of trace metals: Fundamental review” [Advances in Sample Preparation 19, August 2026, 100240] “从胶体到枝晶:二氧化硅纳米颗粒作为痕量金属分析中样品制备的高级固相萃取吸附剂:基础综述”的勘误表[样品制备进展19,20268,100240]
IF 6.6
Advances in Sample Preparation Pub Date : 2026-08-01 DOI: 10.1016/j.sampre.2026.100242
Khaled M. AlMohaimadi, Awadh O. AlSuhaimi
{"title":"Corrigendum to “From colloids to dendrites: Silica nanoparticles as advanced solid-phase extraction sorbents for sample preparation in the analysis of trace metals: Fundamental review” [Advances in Sample Preparation 19, August 2026, 100240]","authors":"Khaled M. AlMohaimadi,&nbsp;Awadh O. AlSuhaimi","doi":"10.1016/j.sampre.2026.100242","DOIUrl":"10.1016/j.sampre.2026.100242","url":null,"abstract":"","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"19 ","pages":"Article 100242"},"PeriodicalIF":6.6,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148934994","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Rescuing RNAs from heparin-contaminated blood samples for RNA sequencing 从肝素污染的血液样本中抢救RNA进行RNA测序
IF 6.6
Advances in Sample Preparation Pub Date : 2026-08-01 Epub Date: 2026-08-07 DOI: 10.1016/j.sampre.2026.100245
Min Yang, Xingbiao Yang, Tao Liu, Qian Luo, Lingyu Liu, Ya Zhang, Meng Wang, Ting Zhang, Nan Zhang, Zhengqiang Guo, Yaolei Zhang, Zeli Luo, Jian Feng
{"title":"Rescuing RNAs from heparin-contaminated blood samples for RNA sequencing","authors":"Min Yang,&nbsp;Xingbiao Yang,&nbsp;Tao Liu,&nbsp;Qian Luo,&nbsp;Lingyu Liu,&nbsp;Ya Zhang,&nbsp;Meng Wang,&nbsp;Ting Zhang,&nbsp;Nan Zhang,&nbsp;Zhengqiang Guo,&nbsp;Yaolei Zhang,&nbsp;Zeli Luo,&nbsp;Jian Feng","doi":"10.1016/j.sampre.2026.100245","DOIUrl":"10.1016/j.sampre.2026.100245","url":null,"abstract":"<div><div>Pre-analytical variations, particularly apoptotic stress responses in blood samples, remain a critical challenge in transcriptomic data harmonization. A major source of this noise is the interference caused by anticoagulants, specifically heparin, which inhibits downstream enzymatic reactions and induces ex vivo stress artifacts that confound gene expression profiles Unlike traditional immediate lysis methods, our approach introduces lithium chloride (LiCl) prior to sample storage to exert a protective effect that mitigates stress-induced cellular damage and reduces apoptosis. Furthermore, LiCl is applied again prior to the RNA precipitation step to serve as a decontamination agent. This LiCl-based protocol is particularly effective for rescuing archived blood samples contaminated with heparin and stored under long-term frozen conditions (-80 °C for up to 180 days). Key results demonstrate that LiCl treatment significantly restores RNA integrity (P &lt; 0.01), achieving an average RIN value &gt; 7.0. Notably, we observed that adding LiCl during the storage of hypoxia-stressed whole blood samples significantly reduced cell apoptosis (P &lt; 0.001). Consequently, little inter-sample variability was observed, and the transcriptomic profiles of rescued samples show high concordance with those from EDTA-anticoagulated controls, enabling high-quality sequencing without the need for complex computational normalization. Thus, this LiCl-based method offers a robust, cost-effective, and environmentally friendly alternative for high-fidelity blood transcriptomics, especially valuable for precious clinical cohorts where re-sampling is not feasible. However, due to LiCl's selective precipitation of larger RNA fragments (&gt;200 nt), this protocol is not suitable for analyses targeting small RNAs such as microRNAs.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"19 ","pages":"Article 100245"},"PeriodicalIF":6.6,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148731378","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Advances in sulfur species analysis in geological materials: methods, challenges, and future directions 地质物质中硫的分析进展:方法、挑战和未来方向
IF 6.6
Advances in Sample Preparation Pub Date : 2026-08-01 Epub Date: 2026-08-10 DOI: 10.1016/j.sampre.2026.100246
Tumelo M Mogashane, Moshalagae A Motlatle, Lebohang V Mokoena, James Tshilongo
{"title":"Advances in sulfur species analysis in geological materials: methods, challenges, and future directions","authors":"Tumelo M Mogashane,&nbsp;Moshalagae A Motlatle,&nbsp;Lebohang V Mokoena,&nbsp;James Tshilongo","doi":"10.1016/j.sampre.2026.100246","DOIUrl":"10.1016/j.sampre.2026.100246","url":null,"abstract":"<div><div>Sulfur has a significant impact on environmental geochemistry, mineral formation, magmatic evolution and biogeochemical cycling, among other geological processes. Accurate identification and quantification of sulfur species in geological materials remain analytically challenging due to their complex mineral matrix, variable oxidation states, and susceptibility to change during sample preparation. This review offers a thorough evaluation of current developments in the investigation of sulfur species in a variety of geological materials, such as rocks, ores, sediments, and fluid inclusions. The strengths, limitations, and analytical performance of several established and emerging techniques, including X-ray Absorption Spectroscopy (XANES/EXAFS), Electron Probe Microanalysis (EPMA), Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS), Ion Chromatography-High-Performance Liquid Chromatography (IC-HPLC), combustion-based methods, Raman spectroscopy, and synchrotron-based microanalytical tools were assessed. The preservation of oxidation states, detection limits, matrix effects, and method standardization are all given special consideration. To improve accuracy and resolution in sulfur speciation, current trends such as multi-method integration, microscale and nanoscale analytical advancements, and machine learning-assisted data interpretation are explored. Lastly, we highlight important knowledge gaps and suggest future lines of inquiry for improving analytical robustness, creating reference materials, and building high-resolution, non-destructive characterisation procedures. The importance of analytical innovation in advancing our understanding of sulfur behaviour in geological systems and enabling broader applications in geochemical modelling, environmental monitoring, and mineral exploration is highlighted in this review.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"19 ","pages":"Article 100246"},"PeriodicalIF":6.6,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148731377","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Integrated one-pot extraction & derivatization of fatty acids in complex food matrices using a thermomorphic solvent system 用热致溶剂系统对复杂食品基质中脂肪酸的一锅萃取衍生化
IF 6.6
Advances in Sample Preparation Pub Date : 2026-08-01 Epub Date: 2026-07-29 DOI: 10.1016/j.sampre.2026.100244
Kaliyani Wickneswaran, David Köhler, Fatemeh Afzalnia, Gerrit Renner, Torsten C. Schmidt
{"title":"Integrated one-pot extraction & derivatization of fatty acids in complex food matrices using a thermomorphic solvent system","authors":"Kaliyani Wickneswaran,&nbsp;David Köhler,&nbsp;Fatemeh Afzalnia,&nbsp;Gerrit Renner,&nbsp;Torsten C. Schmidt","doi":"10.1016/j.sampre.2026.100244","DOIUrl":"10.1016/j.sampre.2026.100244","url":null,"abstract":"<div><div>Conventional lipid extraction workflows (e.g., Folch or Bligh-Dyer) remain difficult to integrate into high-throughput automation because they rely on centrifugation, manual phase handling, and labor-intensive solvent-transfer steps. This study introduces a streamlined one-pot thermomorphic workflow that addresses these bottlenecks by exploiting the temperature-programmed phase behavior of a cyclohexane/methanol system with a literature upper critical solution temperature (UCST) of 45.5°C at x(MeOH) = 0.506. Heating above the UCST enables simultaneous thermal extraction and acid-catalyzed transesterification in a homogeneous single phase. Passive cooling then regenerates the biphasic state, partitioning fatty acid methyl esters (FAMEs) into a directly injectable cyclohexane-rich upper phase for gas chromatography–tandem mass spectrometry (GC–MS/MS) without centrifugation, solvent transfer, or evaporative concentration.</div><div>The selected operating point (65°C, 20 min, φ = 0.50, defined before acetyl chloride addition) was obtained from multivariate screening with an inter-replicate relative standard deviation (RSD) of 2.45%. Calibration yielded linear responses for ten target FAMEs (R² ≥ 0.9672), with limits of detection of 0.070–2.3 mg L⁻¹ and limits of quantification of 0.24–7.8 mg L⁻¹. BCR-162R provided analyte-specific spike-recovery data for five C16–C18 FAMEs, with strongest agreement for C18:2n6-ME and defined limitations for C18:0-ME, C18:1n9-ME, and C18:3n3-ME. Application to six commercial food matrices demonstrated operational feasibility but also matrix- and target-panel-dependent quantitative limitations. NIST SRM 3275 defined the applicability boundary for long-chain polyunsaturated fatty acids (LC-PUFAs) in marine oil. AGREEprep benchmarking gave scores of 0.46 (default) and 0.64 (context-adjusted), indicating a resource-efficient, automation-compatible alternative to conventional lipid sample-preparation workflows.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"19 ","pages":"Article 100244"},"PeriodicalIF":6.6,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148731380","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
In-situ modified polyamide 6 nanofibers for spin-filter solid phase extraction: Effect of azo dye coating on extraction efficiency 原位改性聚酰胺6纳米纤维用于自旋过滤固相萃取:偶氮染料涂层对萃取效率的影响
IF 6.6
Advances in Sample Preparation Pub Date : 2026-08-01 Epub Date: 2026-07-14 DOI: 10.1016/j.sampre.2026.100241
Lucie Chocholoušová Havlíková, Petr Chocholouš, Jakub Erben, Pavel Holec, František Švec, Dalibor Šatínský
{"title":"In-situ modified polyamide 6 nanofibers for spin-filter solid phase extraction: Effect of azo dye coating on extraction efficiency","authors":"Lucie Chocholoušová Havlíková,&nbsp;Petr Chocholouš,&nbsp;Jakub Erben,&nbsp;Pavel Holec,&nbsp;František Švec,&nbsp;Dalibor Šatínský","doi":"10.1016/j.sampre.2026.100241","DOIUrl":"10.1016/j.sampre.2026.100241","url":null,"abstract":"<div><div>Due to their significant surface area and tunable surface chemistry, polymer nanofibers are promising advanced sorbents for miniaturized solid phase extraction of a broad range of model analytes that differ in chemical structures and physical properties. In this study, in-situ modified and coated polyamide 6 nanofibers were evaluated as sorbents for spin-filter solid phase extraction. The modified nanofibers were produced by electrospinning from polymer solutions containing either 3-[dodecyl(dimethyl)ammonio]-1-propanesulfonate (sulfobetaine 12) or tetramethylammonium chloride. Alternatively, the nanofibers were coated with sulfonated azo dyes. This surface modification of nanofibers was identified as a key factor in governing sorbent performance, and led to significantly enhanced extraction efficiency compared to native and uncoated materials. Among the tested sorbents, tartrazine-coated nanofibers exhibited the highest extraction efficiency, particularly for phenolic acids and non-steroidal anti-inflammatory drugs. Recoveries exceeded 90% for most analytes. The developed spin-filter solid phase extraction method coupled with ultra-high performance liquid chromatography with spectrophotometric detection showed good accuracy (85.8–106.6%) and precision (RSD ≤ 4.7%). Applying the method to analyze river water confirmed the suitability of the sorbent for extracting polar xenobiotics prior to chromatographic analysis.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"19 ","pages":"Article 100241"},"PeriodicalIF":6.6,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148642373","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
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