Advances in Sample Preparation最新文献

{"title":"Recent progress in solid- and liquid-phase microextraction methods for the extraction and quantification of current-use pesticides","authors":"Seyedeh Bentolhoda Hosseinian ,&nbsp;Milad Ghani ,&nbsp;Jahan Bakhsh Raoof","doi":"10.1016/j.sampre.2025.100215","DOIUrl":"10.1016/j.sampre.2025.100215","url":null,"abstract":"<div><div>The widespread use of pesticides has led to their pervasive presence in diverse environmental matrices such as water, air, and soil. Therefore, accurate and reliable determination of pesticides in various sample types is essential. In recent years, a range of miniaturized extraction techniques, particularly solid-phase microextraction (SPME) and liquid-phase microextraction (LPME), have been developed. This review provides a comprehensive overview of recent advancements in liquid- and solid-phase microextraction techniques for separation and quantification of pesticides, while also critically evaluating their respective advantages and limitations. In addition, different configurations of solid- and liquid phase microextraction used for the extraction of pesticides are discussed. Moreover, various advanced materials such as molecularly imprinted polymers (MIPs), metal–organic frameworks (MOFs), 3D printed devices, Mxenes, and biopolymers used for the microextraction of pesticides were also discussed.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100215"},"PeriodicalIF":6.5,"publicationDate":"2025-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145220434","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":"Comparison of biodegradable polycaprolactone nanofibers and synthetic polyamide nanofibers as a novel, sustainable sorbent for a spin filter microextraction of xenobiotics from river water","authors":"Ewelina Czyz ,&nbsp;Karolína Macháčková ,&nbsp;Jakub Erben ,&nbsp;Pavel Holec ,&nbsp;František Švec ,&nbsp;Dalibor Šatínský","doi":"10.1016/j.sampre.2025.100214","DOIUrl":"10.1016/j.sampre.2025.100214","url":null,"abstract":"<div><div>We evaluated the application of nanofibers made from different biodegradable and synthetic polymers as sorbents in a new technique of spin filter fiber-microextraction. Biodegradable polycaprolactone fibers, produced via the meltblowing process exhibited robust hydrophobic interactions with lipophilic analytes and were the most effective. The highly porous and permeable structure of the fibrous material ensured exhaustive extraction of xenobiotics from river water. Recovery rates ranged from 81.8 to 105.2 %, except for 4-nitrophenol, a more polar analyte, for which the recovery was 60 %. Only 10 s were needed for activation, extraction, and elution, significantly reducing the time required to complete the procedure in only 30 s per sample. Our method exhibited excellent analytical performance, achieving linearity in the range of 50–2000 µg L⁻¹ for most analytes (100–2000 µg L⁻¹ for PNP and 2-CP; and 100–1000 µg L⁻¹ for PER) with a coefficient of determination (R²) greater than 0.9952. The limits of detection were recalculated based on the slope of the calibration curves and the standard deviation of six replicate measurements at the lowest calibration point for each analyte, yielding values in the range of 7.0–36.6 µgL^-1. Repeatability between extractions (i.e. inter-extraction precision) was evaluated by performing six parallel runs using different cartridges (<em>n</em> = 6). The obtained RSD precision values ranged from 2.2 to 3.3 % demonstrating the excellent uniformity of the nanofibrous materials filled in the devices . We also assessed the reusability of the individual cartridges by performing six consecutive extractions on the same spin filter (i.e. intra-cartridge precision, <em>n</em> = 6), yielding RSD values between 1.1 and 3.6 %. These results confirm that the spin filters cartridges filled with polycaprolactone nanofibers can be effectively reused for multiple extractions in absence of sample carry-over effect.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100214"},"PeriodicalIF":6.5,"publicationDate":"2025-09-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145109727","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":"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 ,&nbsp;María Luisa Marina ,&nbsp;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 3² design) were employed to maximize the recovery of proteins, antioxidants, and antimicrobial compounds, while minimizing the formation of potentially harmful Maillard products during extraction. HIFU demonstrated a greater capability for extracting proteins, which increased significantly when combined with EAE using a polysaccharidase enzyme. The largest protein extraction was achieved from the ginger extract using HIFU for 18 min, at 60 ºC and 80 % amplitude, combined with EAE using Celluclast enzyme. The extracts obtained using SWE showed significant antioxidant activity, with a slight improvement observed when using 2 cycles instead of one. The highest antioxidant activity was observed in the extract obtained from the turmeric waste using SWE at 175 ºC for 15 min. The extracts also exhibited antimicrobial activity, especially against <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":"2025-09-13","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}

{"title":"Versatile sorbent materials in sample preparation: Where do we go next?","authors":"Rafael Oliveira Martins,&nbsp;Maria Flávia Assunção Magalhães,&nbsp;Winnie Evelyn Valeria Perez Vite,&nbsp;Jussara da Silva Alves,&nbsp;Camila Will,&nbsp;Fernando Mauro Lanças","doi":"10.1016/j.sampre.2025.100211","DOIUrl":"10.1016/j.sampre.2025.100211","url":null,"abstract":"<div><div>Continuous advances in sample preparation methods have led to the development of enhanced strategies to address the complexity of diverse matrices in both qualitative and quantitative analyses. These methods are designed to facilitate sample clean-up and preconcentration of target analytes before analysis by different analytical instruments. In both conventional and miniaturized solid-based approaches, the analytical performance of the extraction is primarily influenced by the sorbent phase. As the sorbent is responsible for mediating the interaction between the target analytes and the extraction material, careful selection is essential. In this context, a wide range of sorbent materials has been introduced to ensure efficient and selective interactions, supporting their application in sample preparation protocols. Nevertheless, the literature still lacks comprehensive and up-to-date reviews that highlight recent advances in sorbent development, including both conventional and bio-based alternatives. Therefore, this review aims to provide a current overview of sorbent innovations, discuss emerging trends, and outline potential future directions in the field.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100211"},"PeriodicalIF":6.5,"publicationDate":"2025-09-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145010830","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":"Investigating the impact of novel brominated flame retardants (NBFRs) on metabolite and nutritional profiles in aquatic organisms by in vivo solid-phase microextraction (SPME)","authors":"Tianning Chen ,&nbsp;Pengfei Ye ,&nbsp;Chen Yuan ,&nbsp;Ling Fang ,&nbsp;Nan Li ,&nbsp;Guosheng Chen ,&nbsp;Junlang Qiu ,&nbsp;Fang Zhu ,&nbsp;Gangfeng Ouyang","doi":"10.1016/j.sampre.2025.100212","DOIUrl":"10.1016/j.sampre.2025.100212","url":null,"abstract":"<div><div>Novel brominated flame retardants (NBFRs), due to their ubiquitous environmental distribution in aquatic ecosystems and potential adverse effects to aquatic biota, have initiated global concerns. NBFRs were absorbed and bioaccumulated into aquatic organisms, impairing their growth while significantly disrupting metabolic and nutritional profiles deserves further elucidation, especially for in vivo and in situ characterization. In this study, we selected tilapia (Oreochromis mossambicus) as a model and developed an innovative in vivo sampling method using solid-phase microextraction (SPME) with a cationic covalent organic framework (COF) coating fiber, coupled with high performance liquid chromatography-electrospray ionization-Orbitrap mass spectrometry (HPLC-ESI-Orbitrap-MS) analysis. Our results demonstrated that self-made SPME fibers possessed excellent broad-spectrum extraction ability (totally 5250 molecular features were detected), and the developed analysis method has the advantages of greenness. SPME technology based on our self-made fiber was successfully applied in research of the impacts of NBFRs on tilapia. After statistical analysis, a total of 811 metabolites exhibited significant differential expression, including the nutritional components such as amino acids, glycosides, and lipids, which resulted in a decline in nutritional quality. These findings provided a new perspective for evaluating the ecological risk assessment of NBFRs, nutritional quality assessment of aquatic organisms and securing fishery products.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100212"},"PeriodicalIF":6.5,"publicationDate":"2025-09-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145027128","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":"In-situ simultaneous extraction of non-steroidal anti-inflammatory drugs from wastewater using 3D-printed device and UHPLC-DAD/FLD analysis","authors":"César Castro-García ,&nbsp;Arianna Palermo ,&nbsp;Edwin Palacio ,&nbsp;Luz O. Leal ,&nbsp;Laura Ferrer","doi":"10.1016/j.sampre.2025.100210","DOIUrl":"10.1016/j.sampre.2025.100210","url":null,"abstract":"<div><div>Non-steroidal anti-inflammatory drugs (NSAIDs) are widely employed in medicine for their anti-inflammatory and antipyretic properties. Their occurrence has been documented in effluents from wastewater treatment plants (WWTPs), as well as in aquatic ecosystems. NSAIDs are classified as emerging contaminants, thereby underscoring the importance of their environmental monitoring. This study presents a novel approach for the simultaneous on-site extraction of six NSAIDs –acetylsalicylic acid (ASP), celecoxib (CEL), diclofenac (DIC), ibuprofen (IBU), ketoprofen (KET), and naproxen (NAP)– from wastewater, followed by ultra-high performance liquid chromatography coupled with photodiode array and fluorescence detection (UHPLC-DAD/FLD). A 3D-printed device, coated with a highly selective solid-phase extraction (SPE) resin (Oasis HLB®), enabled on-site extraction and preconcentration of the analytes, avoiding to handle large sample volumes. A peristaltic pump helps both retention and elution steps. Method detection limits were 0.12 µg L^-1 for ASP, 0.16 µg L^-1 for CEL and IBU, 1.5 µg L^-1 for DIC, 0.09 µg L^-1 for KET and 0.19 µg L^-1 for NAP. The analytical performance of the 3D-printed device was demonstrated by precision below 5 % and the possibility of reusing up to 24 times without significant loss of extraction efficiency. An AGREEprep score of 0.53 classifies this methodology as moderately green. On-site analysis was conducted at the Calvià WWTP (Mallorca, Spain), where five NSAIDs were detected at various stages, demonstrating the feasibility of the on-site extraction across a broad concentration range. Except for ASP, which exhibited a recovery rate below 47 %, the remaining analytes showed satisfactory recoveries, ranging from 90 to 98 %.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100210"},"PeriodicalIF":6.5,"publicationDate":"2025-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144989916","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":"Paper as an ecodesigned and smart material for sample preparation integrated with electrochemical (bio)sensors","authors":"Vincenzo Mazzaracchio ,&nbsp;Christian Gosti ,&nbsp;Laura Belcastro ,&nbsp;Fabiana Arduini","doi":"10.1016/j.sampre.2025.100207","DOIUrl":"10.1016/j.sampre.2025.100207","url":null,"abstract":"<div><div>Since 2009, paper-based electrochemical biosensors have demonstrated several additional features in analytical chemistry thanks to their capability to manage the fluids by pump-free microfluidics, easily preconcentrate the target analytes, treat the sample with a task-free approach, and detect the target analyte with high sensitivity and accuracy. Herein, we point out the use of paper as a functional material for sample preparation, addressing easily and in a sustainable way the fluid sample management, filtration, separation, centrifugation, chemical sample treatment, and reagent addition. The use of paper for sample preparation in the electrochemical (bio)sensor field is shed light for the first time in a dedicated review. The overriding goal is to highlight the advantages of these cost-effective, environmentally friendly, and easy-to-use devices for smart preparation procedures and accurate electrochemical detection of the target analytes in several fields, including biomedical, environmental, and agrifood.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"16 ","pages":"Article 100207"},"PeriodicalIF":6.5,"publicationDate":"2025-08-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144989996","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":"Advanced solid materials for the extraction of drugs from biological fluids","authors":"P. García-Atienza,&nbsp;A. García-Juan,&nbsp;S. Armenta,&nbsp;J.M. Herrero-Martínez,&nbsp;H. Martínez-Pérez-Cejuela","doi":"10.1016/j.sampre.2025.100202","DOIUrl":"10.1016/j.sampre.2025.100202","url":null,"abstract":"<div><div>The determination of drugs in biological fluids is essential across various fields, including toxicological analysis, pharmacokinetic studies, and the development of new pharmaceutical products, among others. However, the complexity of biological matrices—due to the presence of endogenous compounds and the typically low concentrations of target analytes—needs efficient sample preparation strategies alongside high-performance instrumentation to achieve the sensitivity and selectivity required in modern analytical chemistry. In response to these challenges, recent advancements have focused on the development of advanced solid materials and their integration with sample preparation techniques. This review highlights recent progress in sorbents with enhanced selectivity, engineered materials such as crystalline frameworks, and the use of biopolymers as natural sorbents for drug analysis in biofluids. Additionally, the application of 3D-printed materials for the fabrication of extraction devices is presented. The article also provides insights into emerging trends and future directions in this evolving field.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100202"},"PeriodicalIF":6.5,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144749610","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":"Greenness of extraction procedures involving biochar-based sorbents for organic compounds","authors":"Francesca Merlo,&nbsp;Andrea Speltini,&nbsp;Antonella Profumo","doi":"10.1016/j.sampre.2025.100203","DOIUrl":"10.1016/j.sampre.2025.100203","url":null,"abstract":"<div><div>In the field of green sample preparation, new challenges are emerging for guaranteeing sustainability of analytical procedures and remarkable efforts have been made to develop materials from natural and/or renewable sources. In such a scenario, biochar is emerging as alternative sorbent with low economic and environmental impact. It is a carbon-rich material derived from the thermochemical conversion of biomass and waste and endowed with excellent textural properties such as high specific surface area and meso‑ and microporosity, and functional groups that are fundamental for the sorption behaviour, a key point in the analytical performance of biochar. These outstanding properties generated a growing interest in the use of biochar-based sorbents in sample preparation. In this context, this review provides an overview of the last 4-year applications of biochar in extraction techniques through an evaluation of greenness of the sample preparation procedures. At this purpose, two metric tools specific for the sample preparation, as AGREEprep and Sample Preparation Metric of Sustainability (SPMS), have been selected to give comprehensive evaluations about greenness, considering multiple criteria but with different weights and intervals in the parameters. Indeed, the papers here reviewed received in SPMS scores ranging from 5.16 to 10, and in AGREEprep from 0.16 to 0.7, evidencing there is space for improving extraction procedures involving biochar-based sorbents.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100203"},"PeriodicalIF":6.5,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144749611","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":"Multiple-shell amorphous Co/Ni-(PO4)x(OH)y hollow layered double hydroxide for enhanced extraction of some azole antifungals from biological samples","authors":"Maedeh Saadat,&nbsp;Yadollah Yamini","doi":"10.1016/j.sampre.2025.100209","DOIUrl":"10.1016/j.sampre.2025.100209","url":null,"abstract":"<div><div>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.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100209"},"PeriodicalIF":6.5,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144925091","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}