Advances in Sample Preparation最新文献

{"title":"Development of smart samplers and their comparison to dried serum spots for the analysis of growth hormone releasing hormone analogs using LCHRMS/MS","authors":"Christina Johannsen ,&nbsp;Anna Kha Tu Nguyen ,&nbsp;Sasha Shabani ,&nbsp;Inger Oulie ,&nbsp;Siri Dørum ,&nbsp;Yvette Dehnes ,&nbsp;Leon Reubsaet ,&nbsp;Trine Grønhaug Halvorsen","doi":"10.1016/j.sampre.2025.100190","DOIUrl":"10.1016/j.sampre.2025.100190","url":null,"abstract":"<div><div>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.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100190"},"PeriodicalIF":5.2,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144185228","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 sample preparation techniques in food analysis: the rise of compressed fluids and novel solvents","authors":"Luana C. dos Santos ,&nbsp;Juan Felipe Grisales-Mejía ,&nbsp;Monique Martins Strieder ,&nbsp;Jose A. Mendiola ,&nbsp;Elena Ibáñez","doi":"10.1016/j.sampre.2025.100191","DOIUrl":"10.1016/j.sampre.2025.100191","url":null,"abstract":"<div><div>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.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100191"},"PeriodicalIF":5.2,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144168993","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":"Progress in functional covalent organic frameworks as advanced materials for sample pretreatment","authors":"Hui Cao ,&nbsp;WeiKang Guo ,&nbsp;Ke Liu ,&nbsp;Qin Shuai ,&nbsp;Lijin Huang ,&nbsp;Zhaochu Hu","doi":"10.1016/j.sampre.2025.100200","DOIUrl":"10.1016/j.sampre.2025.100200","url":null,"abstract":"<div><div>Covalent organic frameworks (COFs) represent an emerging class of porous crystalline materials with immense potential as advanced materials for sample pretreatment. Their distinctive characteristics, including large specific surface areas, adjustable pore structures, robust chemical stability, and abundant active sites, render them a reliable platform for efficiently extracting analytes, thereby opening avenues for innovative applications in analytical chemistry. This review focuses on recent research progress in the utilization of functional COFs for the preconcentration of contaminants, including organic pollutants (such as drugs, pesticides, and dyes) and heavy metal ions. COFs featuring diverse functional groups, such as carboxyl, sulfonyl, hydroxyl, amino, nitro and halogen moieties and their integration with advanced sample pretreatment techniques are discussed. The review begins by examining two primary strategies for functionalizing COF: \"bottom-up\" and \"post-synthetic modification\". Subsequently, the interaction mechanisms and analytical performances of methods based on functionalized COFs are critically analyzed, emphasizing their extraction efficiency and selectivity. Finally, the technical merits of functional COFs as high-performance adsorbents in sample pretreatment are highlighted, while addressing current challenges and outlining future research directions. This review aims to provide a comprehensive reference for the rational design and practical applications of functionalized COFs in advanced sample pretreatment workflows.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100200"},"PeriodicalIF":5.2,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144663689","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":"Pretreat immunosuppressants in whole blood without vortexing and centrifugation","authors":"Rui Zhang ,&nbsp;Ren-Jie Yang ,&nbsp;Ping-An Zhang ,&nbsp;Shao-Ting Wang","doi":"10.1016/j.sampre.2025.100198","DOIUrl":"10.1016/j.sampre.2025.100198","url":null,"abstract":"<div><h3>Background</h3><div>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.</div></div><div><h3>Results</h3><div>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 (<em>n</em> = 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.</div></div><div><h3>Significance</h3><div>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.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100198"},"PeriodicalIF":5.2,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144595951","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":"Advances in magnetic nanomaterials for biomedical sample pretreatment: synthesis, functionalization, and applications in magnetic solid-phase extraction","authors":"Jiarui Zhang ,&nbsp;Shuang Feng ,&nbsp;Yalin Xi ,&nbsp;Meiyun Shi ,&nbsp;Lei Yin","doi":"10.1016/j.sampre.2025.100208","DOIUrl":"10.1016/j.sampre.2025.100208","url":null,"abstract":"<div><div>Magnetic nanomaterials (MNMs) are highly effective sorbents for biomedical sample pretreatment, leveraging their superparamagnetism, large specific surface area, and tunable surface functionalities. This review comprehensively examines MNM classification, synthesis techniques, and functionalization approaches, highlighting their pivotal role in magnetic solid-phase extraction (MSPE) for analyte enrichment. We systematically detail MNM applications in biomedical sample processing, focusing on MSPE for efficient nucleotide isolation, specific protein capture, and ultrasensitive biomarker detection. While MNM-based MSPE offers significant advantages in sensitivity, selectivity, and operational simplicity, challenges remain in achieving reproducible synthesis and deepening the mechanistic understanding of adsorption processes. Future research should prioritize developing automated MSPE platforms and multifunctional MNMs capable of addressing complex clinical matrices. This work provides a valuable reference for designing next-generation analytical systems utilizing MNMs.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100208"},"PeriodicalIF":6.5,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144903830","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}

{"title":"Supported liquid membrane-coupled Extraction","authors":"Shengjie Hu ,&nbsp;Xiantao Shen ,&nbsp;Chuixiu Huang","doi":"10.1016/j.sampre.2025.100197","DOIUrl":"10.1016/j.sampre.2025.100197","url":null,"abstract":"<div><div>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.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100197"},"PeriodicalIF":5.2,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144632451","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":"Green solvents and enzymes combined with advanced extraction techniques for the recovery of bioactive carotenoids and extractable/non-extractable polyphenols from grapefruit peels","authors":"Gloria Domínguez-Rodríguez ,&nbsp;María Concepción García ,&nbsp;María Luisa Marina","doi":"10.1016/j.sampre.2025.100192","DOIUrl":"10.1016/j.sampre.2025.100192","url":null,"abstract":"<div><div>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.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100192"},"PeriodicalIF":5.2,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144240816","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":"Enhanced electromembrane extraction of acidic drugs using a chitosan-agarose hybrid gel membrane","authors":"Hasti Gharah Sheikhlou ,&nbsp;Majid Gharah Sheikhlou ,&nbsp;Marzieh Saberi ,&nbsp;Saeed Nojavan","doi":"10.1016/j.sampre.2025.100196","DOIUrl":"10.1016/j.sampre.2025.100196","url":null,"abstract":"<div><div>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.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100196"},"PeriodicalIF":5.2,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144570583","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":"Recent green approaches in liquid-phase microextraction","authors":"Miguel Ángel Aguirre ,&nbsp;Natalia Arroyo-Manzanares ,&nbsp;Laura Carbonell-Rozas ,&nbsp;José Grau ,&nbsp;Carlos Moreno ,&nbsp;Lorena Vidal","doi":"10.1016/j.sampre.2025.100201","DOIUrl":"10.1016/j.sampre.2025.100201","url":null,"abstract":"<div><div>The miniaturization of conventional extraction techniques, particularly microextraction methods, has led to a reduction in the use of hazardous reagents and waste. However, the continued use of toxic solvents and materials, along with time-consuming sample preparation processes, negatively impacts the overall sustainability of these methods. As a result, there is growing interest in exploring greener alternatives. This review highlights the most promising green solvents for liquid-phase microextraction, including (natural) deep eutectic solvents, low-toxicity ionic liquids, surfactants, micellar solvents, and bio-based solvents, emphasizing their applications in innovative sample preparation techniques in the last five years. Particular emphasis is placed on their use in automated and semi-automated systems, in line with the increasing role of automation in Analytical Chemistry. Selected applications have been carefully reviewed and discussed to illustrate key advances in the use of green solvents and automation for extracting a wide range of compounds from various matrices. In addition, future perspectives are outlined to guide further development of liquid-phase microextraction in alignment with current trends in green sample preparation.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"15 ","pages":"Article 100201"},"PeriodicalIF":5.2,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144685863","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}