Tar Tar Moe Htet, David J. Cocovi-Solberg, Hana Sklenářová, Burkhard Horstkotte
{"title":"Lab-in-syringe automated sample preparation including deproteination, analyte extraction, and solvent evaporation coupled online to HPLC for the determination of water-soluble vitamins in plant-based milk alternatives","authors":"Tar Tar Moe Htet, David J. Cocovi-Solberg, Hana Sklenářová, Burkhard Horstkotte","doi":"10.1016/j.sampre.2026.100243","DOIUrl":"10.1016/j.sampre.2026.100243","url":null,"abstract":"<div><div>Solvent-assisted matrix precipitation, followed by centrifugation, supernatant subtraction, solvent evaporation, and reconstitution, is a commonly used yet laborious procedure for preparing complex sample matrices. Its automation has not yet been tested using flow approaches, despite the potential to save time and consumables and yield higher procedural reproducibility. To tackle this challenging issue, we have developed a Lab-In-Syringe-automated methodology coupled online to HPLC for the determination of water-soluble vitamins B1, B2, B3, B6, B9, and B12 in plant-based milk alternatives.</div><div>Salt-assisted homogeneous liquid-liquid extraction, automated using an automatic syringe pump, was used to simultaneously denature proteins and separate the precipitable sample matrix from oat, soy, hazelnut, almond, and coconut milk substitutes. The organic phase was passed into a secondary, coupled automatic syringe pump that used preheated air for solvent evaporation.</div><div>To the best of our knowledge, this is the first report on combining fully automated matrix precipitation and solvent evaporation in flow techniques. This way, we achieved a significant improvement in analyte concentration compared to earlier reported in-syringe deproteination, where significant extract dilution had been required to achieve compatibility with HPLC.</div><div>Highlighted features include a sub-milliliter sample volume, a total processing time of only 9 min, including intermediate system cleaning, and online coupled HPLC-UV analysis of the extract in parallel with sample processing, yielding a sample throughput of 5/h. Adequate analytical performance for routine analysis was achieved with quantitative protein elimination, LOQs of 0.5–2.7 µg/L, and RSDs of 1.1–2.6 %, < 5% omitting an internal standard. Analysis of milk samples, both genuine and spiked, yielded an average recovery of 92 ± 11 %.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"19 ","pages":"Article 100243"},"PeriodicalIF":6.6,"publicationDate":"2026-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148731379","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}
Mehmet Berk Bilgin , Norma Toccalino , Emma Slack , Adrian Egli , Andreas T. Güntner
{"title":"Bacterial headspace sampler for real-time volatilome monitoring","authors":"Mehmet Berk Bilgin , Norma Toccalino , Emma Slack , Adrian Egli , Andreas T. Güntner","doi":"10.1016/j.sampre.2026.100237","DOIUrl":"10.1016/j.sampre.2026.100237","url":null,"abstract":"<div><div>The bacterial volatilome is rich in information that can be exploited for metabolic investigations and infectious disease diagnostics, including identification and, potentially, rapid antimicrobial susceptibility testing. Robust and reliable headspace sampling is critical for the capture of bacterial emissions. Here, we introduce a standardized bacterial headspace sampling technique for reproducible and real-time analysis of bacterial growth plates. The system is based on an inert volume sampler for the accumulation and triggered extraction of trace-level microbial volatile organic compounds (mVOCs) from inoculated samples under controlled temperature and relative humidity (e.g., 37 °C and 80%, respectively). Integrated sample dilution is achieved using high-resolution mass flow controllers to meet the dynamic range requirements of various analytical tools, for instance, mass spectrometers and chemical sensors. A built-in analyte gas standard enables calibration between measurements. The sampling characteristics are assessed for key mVOCs (acetaldehyde, acetone, benzene, and ethanol) within relevant concentration ranges, down to 50 parts-per-billion by volume (ppb) levels. <em>In vitro</em> tests with DSM 613 <em>Escherichia coli</em> confirm accurate capture of mVOC dynamics reflecting physiological changes during bacterial growth, as monitored by proton transfer reaction time-of-flight mass spectrometry over 24 h. This setup offers a standardized approach compatible with diverse analytical tools for exploring the microbial volatilome.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"18 ","pages":"Article 100237"},"PeriodicalIF":6.5,"publicationDate":"2026-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148184813","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Microwave-assisted extraction of isoangustone A from Derris scandens (Roxb.) Benth. using a hydrophobic deep eutectic solvents-based microemulsion","authors":"Benyatip Buajan , Mudtorlep Nisoa , Fonthip Makkliang , Waraporn Putalun , Geoffrey A. Cordell , Rawiwan Charoensup , Gorawit Yusakul","doi":"10.1016/j.sampre.2026.100232","DOIUrl":"10.1016/j.sampre.2026.100232","url":null,"abstract":"<div><div>The aim of this research was to develop a new extraction method combining hydrophobic deep eutectic solvent (HDES)-based microemulsion systems with microwave-assisted extraction (MAE) technology to enhance the extraction efficiency of isoangustone A (IsoA) from the leaves of the Thai medicinal plant <em>Derris scandens</em> (Roxb.) Benth. (Fabaceae). The research optimized the extraction parameters, characterized the microemulsion formulations, and evaluated the anti-inflammatory potential of the preparations <em>in vitro</em>. The HDES (menthol:lactic acid, 1:2 mol ratio)-microemulsion formulation demonstrated enhanced extraction efficiency over conventional ethanol-based methods. This formulation achieved a yield of IsoA of 6.52 μg/mg, surpassing the 5.76 μg/mg yield obtained through ethanol extraction. Response Surface Methodology (RSM) modeling enabled precise optimization of the extraction parameters, reaching 91.2 % predictive accuracy. Physicochemical characterization revealed that HDES-based microemulsions maintained 23.1–50.7 nm size, facilitating an enhanced bioavailability profile. The incorporation of <em>D. scandens</em> leaf extracts into the HDES (menthol:lactic acid, 2:1 mol ratio)-based microemulsion provided optimal inhibition of LPS-induced NO production in RAW264.7 macrophages, with IC<sub>50</sub> values (9.07±2.26 μg/mL) substantially lower than the DMSO-solubilized counterparts (53.7±3.8 μg/mL) demonstrating enhanced cell penetration resulting in improved extraction. This integrated approach represents a significant advancement in sustainable extraction technology, offering enhanced recovery of bioactive compounds while preserving their biological properties for further assessment.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"17 ","pages":"Article 100232"},"PeriodicalIF":6.5,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147394992","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Innovative ultrasound-assisted and vacuum manifold-assisted pipette tip solid-phase extraction using MSU-2-C18 sorbent for the extraction and purification of glycoalkaloids in potato-based snacks prior to UHPLC-MS/MS analysis","authors":"Isabel Martínez-García , Damián Pérez-Quintanilla , Sonia Morante-Zarcero , Isabel Sierra","doi":"10.1016/j.sampre.2025.100228","DOIUrl":"10.1016/j.sampre.2025.100228","url":null,"abstract":"<div><div>A miniaturized and environmentally conscious analytical workflow was developed and validated for the extraction, purification, and quantification of major glycoalkaloids (α-solanine, α-chaconine), the degradation product γ-chaconine, and the aglycone solanidine in potato-based snack products. The method combines ultrasound-assisted extraction (UAE) with pipette-tip solid-phase extraction (PT-SPE), followed by UHPLC-MS/MS analysis. UAE conditions were optimized using a Box-Behnken statistical design, which evaluated the extraction time, ultrasound amplitude, and solid:liquid (SL) ratio. Optimal conditions were determined to be 5 min, 100 % amplitude, and a 1:9 w/v of SL ratio, with methanol as the most effective extraction solvent. MSU-2-C18 mesostructured silica sorbent, packed into pipette tips (5 mg) connected to a SPE vacuum manifold (VMA-PT-SPE), was employed under the optimized conditions to simultaneously purify up to 12 extracts. The method's greenness was evaluated using the AGREEprep metric, yielding a score of 0.65, indicating good environmental performance. Limits of detection (LOD) and quantification (LOQ), ranging from 0.55–4.40 µg/kg and 1.82–14.67 µg/kg, respectively, were achieved for the target analytes. Application to four commercial potato-based snacks revealed major (α-solanine and α-chaconine) and minor glycoalkaloids (γ-chaconine and solanidine) levels, ranging from 2.0 to 16.0 mg/kg fresh weight, highlighting substantial variability among products and providing a more comprehensive characterization of the glycoalkaloid profile. Compared to conventional SPE formats, this UAE-VMA-PT-SPE strategy offers superior reproducibility while reducing sample and solvent consumption. The method represents a powerful tool for routine monitoring of glycoalkaloids in potato snacks, supporting food safety assessments and addressing analytical priorities established by the European Food Safety Authority.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"17 ","pages":"Article 100228"},"PeriodicalIF":6.5,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145685073","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Electromembrane extraction of tetracyclines in foods and human plasma prior to LC-MS/MS analysis: Impact of sample matrix on extraction performance","authors":"Anne Oldeide Hay, Frederik André Hansen","doi":"10.1016/j.sampre.2025.100227","DOIUrl":"10.1016/j.sampre.2025.100227","url":null,"abstract":"<div><div>Tetracyclines are widely used antibiotics in animal farming, raising concerns over their residues in food and associated health risks. Current methods for residue determination are complex, time-consuming, and produce substantial solvent waste. Electromembrane extraction (EME) offers high clean-up efficiency, minimal solvent use, and direct LC-MS/MS compatibility. This study evaluates EME for extraction of four tetracyclines (oxytetracycline, tetracycline, chlorotetracycline, doxycycline) from complex matrices including milk, egg white, honey, and human plasma. Optimal parameters varied across matrices, underscoring the need for matrix-specific optimization. Optimized methods achieved recoveries of 66–101 %, excellent linearity (R² = 0.9929–0.9998), and minimal matrix effects (-14 % to 1 %). LLOQs ranged from 0.5 to 2.1 ng/g, with calibration curves extending to 1000 ng/g, covering concentrations relevant for residue monitoring. These results demonstrate EME’s potential for reliable analysis of challenging polar and zwitterionic compounds in food and biological samples. Finally, the greenness was evaluated by the AGREEprep metric tool, gaining a total score of 0.64.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"17 ","pages":"Article 100227"},"PeriodicalIF":6.5,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145610426","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Ewelina Czyz , Marie Štorková , Jakub Erben , Pavel Holec , František Švec , Dalibor Šatínský
{"title":"Hydrophobic and aromatic polymer nanofibers for a spin-filter micro solid phase extraction of polycyclic aromatic hydrocarbons in river water","authors":"Ewelina Czyz , Marie Štorková , Jakub Erben , Pavel Holec , František Švec , Dalibor Šatínský","doi":"10.1016/j.sampre.2026.100229","DOIUrl":"10.1016/j.sampre.2026.100229","url":null,"abstract":"<div><div>The use of hydrophobic and aromatic polymer nanofibers as novel sorbents for extracting polycyclic aromatic hydrocarbons (PAHs) from river water has been evaluated. Of the materials tested, the biodegradable aliphatic polymer polycaprolactone (PCL) exhibited strong retention of all analytes via hydrophobic interactions. In contrast, the aromatic polymer polyphenylene sulfide (PPS) demonstrated superior performance with higher-ring PAHs due to a combination of hydrophobic and π–π stacking interactions. The porous, permeable structure of the fibrous sorbents enabled rapid extraction. The spin-filter µSPE format required only 10 s for sorbent activation, extraction, and elution, resulting in a total processing time of 30 s per sample. Up to 48 samples could be processed simultaneously, reducing manual handling and simplifying the workflow. Analytical performance was evaluated using river water spiked at different concentration levels. The method showed good linearity (R² ≥ 0.98) across concentration ranges of 0.1–5 µg L⁻¹ for most analytes, with limits of detection of 0.009–0.14 µg L⁻¹ for PCL and 0.012–0.27 µg L⁻¹ for PPS. Recoveries ranged from 57 to 102 % for PCL and 88–139 % for PPS, with relative standard deviations below 15 %, and preconcentration factors of approximately twofold. These results demonstrate that meltblown PCL and PPS nanofibers combined with spin-filter µSPE provide a rapid and practical approach to extracting PAHs from environmental water samples.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"17 ","pages":"Article 100229"},"PeriodicalIF":6.5,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146077374","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Gong Zhang , Adam Wawrzynczak , Grace Tseng , Amélie Blais , Andy Nong , Azam F. Tayabali , Guillaume Pelletier , Allison Loan , David Prescott , Kristin M. Eccles , Rocio Aranda-Rodriguez
{"title":"A novel automated micro solid phase extraction (µSPE) method to quantify 21 per- and polyfluoroalkyl substances compounds in biological samples","authors":"Gong Zhang , Adam Wawrzynczak , Grace Tseng , Amélie Blais , Andy Nong , Azam F. Tayabali , Guillaume Pelletier , Allison Loan , David Prescott , Kristin M. Eccles , Rocio Aranda-Rodriguez","doi":"10.1016/j.sampre.2026.100230","DOIUrl":"10.1016/j.sampre.2026.100230","url":null,"abstract":"<div><div>A semi-automated micro solid-phase extraction (μSPE) method has been developed and optimized for the quantification of 21 per- and polyfluoroalkyl substances (PFAS) across various biological matrices, including plasma, serum, urine, and liver tissue. This method employed μSPE cartridges integrated with a PAL-RTC robotic system, which enabled precise flow control and high-throughput procedures while ensuring exceptional extraction efficiency and reproducibility. Sample homogenization of liver tissues was achieved by bead-mill technology which eliminated sample cross-contamination and significantly reduced processing time. The extraction efficiency was influenced by the concentration of methanol in the sample, especially for longer-chain PFAS (C9–14). Extraction efficiencies of over 90% extraction were achieved with loading solutions containing 50–60% methanol in plasma and serum, and up to 80% methanol in water samples. The μSPE protocol included two sequential wash steps that provided excellent matrix clean-up, and reduced background signals by over 95% compared to traditional protein precipitation (PP) methods. The µSPE-LC-MS/MS method offers high sensitivity (method detection limits between 0.008 ng/mL and 0.048 ng/mL), along with good recoveries (90.3 to 105.1%), and precision (RSD <10%). It also demonstrated strong agreement with non-certified values of NIST Standard Reference Materials (SRM 1957/1958). The method was successfully used in the analysis of PFAS in human urine and plasma, as well as in mouse liver samples from an <em>in vivo</em> study. The μSPE approach provides a sensitive, reproducible, and automated solution that requires limited biological sample volumes, making it suitable for the analysis of PFAS in biomonitoring and toxicokinetic studies.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"17 ","pages":"Article 100230"},"PeriodicalIF":6.5,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147394986","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Ingrid Hagarová , Vasil Andruch , Alina Kalyniukova
{"title":"Green hydrophobic deep eutectic solvent-based rapid synergistic cloud point extraction and quantification of ultra-trace lead","authors":"Ingrid Hagarová , Vasil Andruch , Alina Kalyniukova","doi":"10.1016/j.sampre.2025.100225","DOIUrl":"10.1016/j.sampre.2025.100225","url":null,"abstract":"<div><div>In this study, a novel and environmentally friendly analytical procedure was developed for the fast separation and preconcentration of ultra-trace levels of lead from water samples at room temperature. The method is based on a hydrophobic deep eutectic solvent–assisted rapid synergistic cloud point extraction (HDES-RS-CPE), followed by electrothermal atomic absorption spectrometry (ETAAS) for quantification. The selected HDES was composed of <span>l</span>-menthol and 1-octanol in a 1:1 molar ratio, while ammonium pyrrolidine dithiocarbamate (APDC) and Triton X-114 were employed as the chelating agent and nonionic surfactant, respectively. Key experimental parameters influencing extraction efficiency were systematically investigated and optimized. Under optimal conditions, the method achieved a limit of detection (LOD) of 0.04 µg/L, a limit of quantification (LOQ) of 0.12 µg/L, and an enrichment factor (EF) of 38, with spike recoveries ranging from 94 % to 104 %. The method’s greenness, practicality and robustness were confirmed using various metrics demonstrated compliance with the principles of Green Analytical Chemistry, highlighting the method’s potential as a sustainable and efficient approach for ultra-trace lead quantification in environmental samples.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100225"},"PeriodicalIF":6.5,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145623498","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Rubio-Marín Carlos , María Luisa Marina , María Concepción García
{"title":"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","authors":"Rubio-Marín Carlos , María Luisa Marina , María Concepción García","doi":"10.1016/j.sampre.2025.100213","DOIUrl":"10.1016/j.sampre.2025.100213","url":null,"abstract":"<div><div>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 3<sup>2</sup> 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 <em>Staphylococcus aureus</em>, 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.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100213"},"PeriodicalIF":6.5,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145106276","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}