Advances in Sample Preparation最新文献

{"title":"Determination of steroid hormones in sea urchins by microwave-assisted extraction and ultrahigh-performance liquid chromatography tandem mass spectrometry","authors":"Irene Rodríguez-de Cos ,&nbsp;Raibel Núñez-González ,&nbsp;Rayco Guedes-Alonso ,&nbsp;Sarah Piaugeard ,&nbsp;María Esther Torres-Padrón ,&nbsp;José Juan Castro-Hernández ,&nbsp;Zoraida Sosa-Ferrera ,&nbsp;José Juan Santana-Rodríguez","doi":"10.1016/j.sampre.2024.100132","DOIUrl":"10.1016/j.sampre.2024.100132","url":null,"abstract":"<div><div>Marine pollution poses significant threats to ecosystems by contaminating habitats and degrading marine life. This involves the need to develop efficient methodologies to evaluate the compounds that affect marine organisms, such as steroid hormones. The study of the presence of these compounds in marine organisms like sea urchins is very interesting given their role as bioindicators because they feed on algae and are constantly in contact with sediments. Given the low concentrations of steroid hormones in marine environments, it is necessary to develop extraction procedures that allow these pollutants to be extracted and preconcentrated before chemical analyses. Of all the extraction methods, microwave-assisted extraction (MAE) has been used for its many advantages compared to traditional extraction techniques, such as easy sample handling or scarce organic solvents use, and for providing very selective extractions. This study presents the novel MAE optimisation for the extraction of 15 hormones, including five oestrogens, three androgens, four progestogens and three glucocorticoids from sea urchin tissues. The extracted hormones were subsequently determined by high-performance liquid chromatography tandem mass spectrometry. To the best of the authors' knowledge, this approach has not been previously developed. To perform extraction optimisation, different variables were studied following factorial experimental designs. The optimised extraction method showed very appropriate analytical parameters, with limits of detection between 0.21 and 20.4 ng·g^-1 for the four families of studied steroid hormones, and recovery extractions over 60 % for most target compounds. After optimisation, the analytical methodology was applied to samples of three different sea urchins species (<em>Arbacia lixula, Paracentrotus lividus, Sphaerechinus granularis</em>) caught in different locations around the Gran Canaria island (Canary Islands, Spain). The results showed the great applicability of the optimised methodology and two target hormones, boldenone and prednisolone, which were quantified in different samples and locations. This indicates the potential of sea urchins as bioindicators of the health of marine ecosystems and of anthropogenic contamination.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"12 ","pages":"Article 100132"},"PeriodicalIF":5.2,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142357856","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}

{"title":"One step derivatization and switchable hydrophilicity solvent-based microextraction for the determination of adamantane analogues in human urine by HPLC-FLD","authors":"Marianna Ntorkou ,&nbsp;Paraskevas D. Tzanavaras ,&nbsp;Constantinos K. Zacharis","doi":"10.1016/j.sampre.2024.100135","DOIUrl":"10.1016/j.sampre.2024.100135","url":null,"abstract":"<div><div>The present study describes an “one-step” derivatization and microextraction using a pH-switchable hydrophilicity solvent for the determination of amantadine and memantine in human urine by liquid chromatography and fluorescence detection. The procedure is based on the derivatization of the analytes with <em>o</em>-phthalaldehyde/<em>N</em>-acetyl cysteine at alkaline conditions in the presence of sodium salicylate as extractant in a homogeneous solution. The liquid-solid transition of salicylic acid was achieved by adding an aliquot of concentrated phosphoric acid that enables efficient dispersion and phase separation in a single step. Due to the moderate melting point of salicylic acid, its solidification is carried out at room temperature without the need for sample cooling. Critical parameters affecting the efficiency of the derivatization reaction and the microextraction performance were investigated and optimized. The fluorescent analyte derivatives were monitored at <em>λ</em>_ex/<em>λ</em>_em = 340/450 nm. The proposed method was validated in terms of specificity, linearity, precision and trueness. The method was linear in the range of 50–2000 ng mL⁻¹ while the intraday and between days precision was less than 13.7% in all cases. The trueness of the method ranged between 87.9 and 113%. The green character and the applicability of the method were assessed using ComplexMoGAPI and BAGI tools. The developed analytical scheme presented satisfactory performance, and it could be applied in the analysis of selected drugs in human urine samples.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"12 ","pages":"Article 100135"},"PeriodicalIF":5.2,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142702241","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}

{"title":"Recent advances in the application of MOFs and COFs composites for sample preparation","authors":"Wei Zhao,&nbsp;Hui Wang,&nbsp;Qihui Sun,&nbsp;Jia Yang,&nbsp;Xiaoyun Liu,&nbsp;Tiantian Si","doi":"10.1016/j.sampre.2024.100138","DOIUrl":"10.1016/j.sampre.2024.100138","url":null,"abstract":"<div><div>Sample preparation, a vital element across analytical procedures, enhances accuracy, sensitivity, and enrichment of trace analytes, widely applied in food safety, environmental analysis, medicine and health. The choice of extraction materials, a pivotal determinant of efficacy, has been advanced by the development of novel materials, driving progress in sample preparation technologies. Metal-organic frameworks (MOFs), covalent-organic frameworks (COFs) and their composites boast exceptional stability, tunable pores, vast specific surface areas, conferring versatility and applicability across diverse sample preparation domains. Here, we have reviewed the preparation strategies for MOFs, COFs, and their hybrid composites, comprehensively introducing the diverse applications of them in sample preparation. Furthermore, the challenges and development trends for sample preparation in combination with the development of materials were summarized and discussed.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"12 ","pages":"Article 100138"},"PeriodicalIF":5.2,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142702242","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}

{"title":"Rapid and sensitive determination of bongkrekic acid with molecularly imprinted polymer-coated wooden-tip electrospray ionization mass spectrometry","authors":"Chunfei Zhong ,&nbsp;Xinyan Li ,&nbsp;Fan Zhang ,&nbsp;Ning Liu ,&nbsp;Jiewei Deng ,&nbsp;Yunyun Yang ,&nbsp;Tiangang Luan","doi":"10.1016/j.sampre.2024.100137","DOIUrl":"10.1016/j.sampre.2024.100137","url":null,"abstract":"<div><div>In this study, a novel methodology has been developed for the rapid and sensitive analysis of bongkrekic acid (BA), a highly toxic bacterial metabolite, using a molecularly imprinted polymer-coated wooden-tip coupled with electrospray ionization mass spectrometry (MIPWT-ESI-MS). A MIPWT solid phase microextraction (SPME) probe specifically tailored for BA was fabricated, by employing dummy template molecules/functional monomers in the imprinting coating modification. This approach exhibits an enrichment factor (EF) of 683 ± 53 for efficient extraction of BA from aqueous matrices, demonstrating the utility of dummy templates in enhancing the selectivity and sensitivity of the MIPWT-ESI-MS method. The analytical performance of the MIPWT-ESI-MS method was evaluated, demonstrating a desirable linear correlation (<em>r</em> = 0.9988), along with remarkable sensitivity by a limit of detection (LOD) and limit of quantitation (LOQ) at 0.05 μg/L and 0.16 μg/L in pure water, respectively. Additionally, the method demonstrated high repeatability with a relative standard deviation (RSD) &lt; 3.9 % (<em>n</em> = 6) and reproducibility with an RSD &lt; 13.4 %. The practical application of the method was confirmed through the successful analysis of real-world samples, including tap water, wastewater from a food processing factory, and the aqueous extracts of food samples, with BA detected at 0.296 µg/L in <em>Tremella</em>. Spiking experiments further validated the accuracy of the method, with recoveries ranging from 81 % to 97 %. This study integrates MIP with ambient mass spectrometry, offering a robust, selective, and sensitive tool for the monitoring of trace BA levels in complex food and environmental samples, contributing significantly to public health safety and food quality control.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"12 ","pages":"Article 100137"},"PeriodicalIF":5.2,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142702854","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}

{"title":"Natural deep eutectic solvents and natural solid biosorbents in microextraction techniques of organic compounds based on chromatographic techniques: A critical review","authors":"Eduardo Carasek ,&nbsp;Lucas Morés ,&nbsp;Natan da Cunha ,&nbsp;Guilherme Leal Branco ,&nbsp;Adriana Neves Dias","doi":"10.1016/j.sampre.2024.100139","DOIUrl":"10.1016/j.sampre.2024.100139","url":null,"abstract":"<div><div>Analytical chemistry has increasingly focused on the environmental impact of its methods, with significant attention given to green principles in sample preparation. Techniques like Solid-Phase Microextraction (SPME), Micro-Solid-Phase Extraction (µ-SPE), Thin-Film Microextraction (TFME), Stir Bar Extraction (SBSE), Bar-Adsorptive Microextraction (BAµE), Disposable Pipette Extraction (DPX), and Rotative Disk Sorptive Extraction (RDSE) represent advancements in solid-phase extraction methods. Meanwhile, methods such as Single Drop Microextraction (SDME), Dispersive Liquid-Liquid Microextraction (DLLME), and Hollow Fiber Liquid-Phase Microextraction (HF-LPME) focus on liquid-phase techniques. Among the green approaches, biosorbents have gained prominence as extractor materials due to their environmental friendliness, renewability, biodegradability, and cost-effectiveness. In liquid-phase extractions, Natural Deep Eutectic Solvents (NADESs) have emerged as promising alternatives to traditional solvents. NADESs offer benefits such as biodegradability, biocompatibility, low toxicity, and affordability, along with ease of synthesis and purification. This review summarizes the application of NADESs and biopolymers, focusing in biosorbents, in microextraction and other techniques, based on literature from 2017 to the present. It is evident that NADESs present viable alternatives to conventional solvents, with their physical-chemical properties like viscosity, density, and polarity, being tunable through various mixtures. Similarly, biosorbents offer unique physicochemical properties that can outperform traditional commercial materials in sample preparation. Applications discussed in this review focus on the determination of organic compounds in environmental, food, and biological samples, utilizing chromatographic methods. These developments highlight the ongoing evolution in green analytical practices, aiming for more sustainable and efficient analytical procedures.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"12 ","pages":"Article 100139"},"PeriodicalIF":5.2,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142748719","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}

{"title":"Simultaneous and sequential combination of techniques for the sustainable and extensive extraction of proteins and polyphenols from malt rootlets","authors":"Ester Hernández-Corroto ,&nbsp;María Luisa Marina ,&nbsp;María Concepción García","doi":"10.1016/j.sampre.2024.100131","DOIUrl":"10.1016/j.sampre.2024.100131","url":null,"abstract":"<div><div>The emergence of tecnhiques such as microwave-assisted extraction (MAE), enzyme-assisted extraction (EAE), ultrasounds-assisted extraction (UAE), and pressurized liquid extraction (PLE) has brough many benefits but their single use does not guarantee the hollistic extraction of target compounds from complex samples. Taking into account their different principles and that one technique may favour the extraction of certain compounds over others, this work proposes the combination of these techniques for improving extraction yields in the recovery of proteins, as example of large molecule, and phenolic compounds, as example of small molecule, from a recalcitrant sample. No single extraction technique recovered all proteins or phenolic compounds, even after a proper optimization. Among them, PLE was the most advantageous, enabling the extraction of 67 % proteins and 1.20 g gallic acid equivalent (GAE)/100 g sample. Analysis of samples by scanning electron microscopy (SEM) and separation of extracts by reversed-phase high performance liquid chromatography (RP-HPLC) and sodium dodecyl sulphate polyacrylamide gel electrophoresis (SDS-PAGE) revealed that PLE showed the most distinct efficiency among EAE, MAE, and UAE, whereas the latter three exhibited more similar results. Based in these results, ten different combinations (sequential and/or simultaneous) of these techniques were proposed. PLE in combination with another technique showed a great potential for the extraction of both large and small molecules. Particularly, the combination of EAE and PLE recovered 100 % of proteins and more than three times the phenolic compounds extracted by other methods reported in the literature, even revealing significant synergistic effects.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"12 ","pages":"Article 100131"},"PeriodicalIF":5.2,"publicationDate":"2024-09-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142320380","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}

{"title":"Improving sample preparation by biochar-coated sampling tubes: proof-of-concept extraction of sex hormones from real waters","authors":"Petra Bianchini,&nbsp;Francesca Merlo,&nbsp;Valentina Quarta,&nbsp;Luca Ferrari,&nbsp;Chiara Milanese,&nbsp;Antonella Profumo,&nbsp;Andrea Speltini","doi":"10.1016/j.sampre.2024.100129","DOIUrl":"10.1016/j.sampre.2024.100129","url":null,"abstract":"<div><div>This work showcases a novel application of biochar for analytical sample treatment. The carbonaceous material, obtained by pyrolysis of orange peel waste (550°C) without any post-synthesis treatment or functionalization, was thoroughly characterized and easily immobilized on the inner wall of sampling tubes in order to perform a sort of “in-vial” solid-phase extraction (SPE). The as-obtained device was tested for the extraction of seven sexual steroids, as probe water pollutants, from tap, lake, river water and wastewater treatment plant effluent samples spiked with 0.2-5 µg L⁻¹ of each compound. The sorption kinetics profiles showed quantitative uptake from the sample (25 mL) in 20 min contact time, followed by complete elution in pure ethanol (2 mL, 15 min), thanks to the proper balance between sorption affinity and ease of elution. Under the selected conditions, recovery was in the range 60-123 %, with good inter-day precision (RSD 10-18 %, <em>n=3</em>). As evidence of the excellent reproducibility, an overall RSD below 15 % was observed from inter-day inter-batch recovery tests on three individually prepared sampling tubes. The procedure, carried out on a roller mixer, allows 10 samples to be extracted simultaneously, improving the sample throughput. Moreover, reusability tests showed that the same device maintains its efficiency for 10 consecutive sorption/desorption cycles. The greenness assessment, carried out by two dedicated software, further supported the sustainability of this biochar-based sample preparation as an alternative SPE.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"12 ","pages":"Article 100129"},"PeriodicalIF":5.2,"publicationDate":"2024-09-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582024000287/pdfft?md5=95668a220309b4dd7509b96413759462&pid=1-s2.0-S2772582024000287-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142312345","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}

{"title":"Green and miniaturized ultrasonic-assisted extraction using natural deep eutectic solvents to extract phenolic compounds from tea samples","authors":"Laura Carbonell-Rozas,&nbsp;Roberto Romero-González,&nbsp;Antonia Garrido Frenich","doi":"10.1016/j.sampre.2024.100128","DOIUrl":"10.1016/j.sampre.2024.100128","url":null,"abstract":"<div><p>Natural deep eutectic solvents (NADES) have emerged as promising green solvents, particularly useful in sample treatment procedures. For the first time, different types of NADES were prepared and evaluated as potential phenolic extraction solvents from tea samples (<em>Camellia sinensis</em>). The NADES, composed of lactic acid:glycerol:water in a molar ratio of 1:1:3, provided the best results for the simultaneous extraction of the target phenolic compounds. This NADES was also characterized by using nuclear magnetic resonance (NMR), and the presence of nuclear Overhauser enhancement effects confirmed its supramolecular structure. The experimental conditions affecting the miniaturized ultrasonic-assisted extraction (UAE) were optimized to maximize extraction efficiency by performing a design of experiments. The proposed sample treatment was combined with ultra-high performance liquid-chromatography coupled to tandem mass spectrometry detection (UHPLC-MS/MS) to determine 21 phenolic compounds including catechin derivatives and other minor compounds. The UAE-UHPLC-MS/MS method was successfully characterized and applied to the analysis of various commercial green, black, white and red tea samples. In all cases, 18 phenolic compounds were determined with concentrations ranging from 0.3 to 29,125 mg kg⁻¹. The proposed sample treatment is a high-throughput, easy, fast and robust alternative to conventional procedures, which reduces organic solvent consumption and costs, aligned with green sample preparation principles.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"12 ","pages":"Article 100128"},"PeriodicalIF":5.2,"publicationDate":"2024-09-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582024000275/pdfft?md5=3b3c736ead7fed8fccc1105929bcf953&pid=1-s2.0-S2772582024000275-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142240990","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}

{"title":"Preconcentration of nanoplastics using micro-electromembrane extraction across free liquid membranes","authors":"Muhandiramge Ranasinghe,&nbsp;Michael C. Breadmore,&nbsp;Fernando Maya","doi":"10.1016/j.sampre.2024.100125","DOIUrl":"10.1016/j.sampre.2024.100125","url":null,"abstract":"<div><p>Asymmetric micro-electromembrane extraction (µ-EME) based on a free liquid membrane has been evaluated for the preconcentration of nanoplastics. A conical unit (200 µL micropipette tip) enabled the simple and reproducible formation of the required three-phase extraction system consisting of a donor solution (150 µL sample/standard solution), free liquid membrane (FLM; 10 µL 1-pentanol), and an acceptor solution (5 µL of 5 mM phosphate buffer, pH 10.7). After µ-EME, nanoplastics transferred across the FLM into the acceptor solution were quantified using capillary zone electrophoresis with diode array detection. Enrichment factors &gt;20 and extraction recoveries &gt;70 % were achieved for nanoplastics concentrated at 500 V during 5 min. The limit of detection (LOD, S/<em>N</em> = 3) and limit of quantification (LOQ, S/<em>N</em> = 10) of the method using 200 nm sulphonated polystyrene particles as model nanoplastics were 6.00×10⁻⁴% (w/v) and 2.00×10⁻³% (w/v), respectively. Intraday (<em>n</em> = 6) and interday (<em>n</em> = 6) repeatability%RSD for 5.5 × 10⁻³% (w/v) nanoplastics were 8.5 % and 7.2 %, respectively. µ-EME enabled an efficient sample matrix clean-up and preconcentration of nanoplastics spiked in tea sample matrices. Nanoplastics preconcentrated through the FLM for black tea resulted in an enrichment factor of 20±3.6 (<em>n</em> = 3), with complete sample matrix removal of UV absorbing compounds.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"11 ","pages":"Article 100125"},"PeriodicalIF":5.2,"publicationDate":"2024-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S277258202400024X/pdfft?md5=36f4203335e30657d3ad7a335a9e9e09&pid=1-s2.0-S277258202400024X-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141997548","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}

{"title":"Electromembrane extraction of human chorionic gonadotropin – A case study on mass transfer of intact protein versus signature peptide","authors":"Torstein Kige Rye ,&nbsp;Frederik André Hansen ,&nbsp;Trine Grønhaug Halvorsen ,&nbsp;Stig Pedersen-Bjergaard","doi":"10.1016/j.sampre.2024.100126","DOIUrl":"10.1016/j.sampre.2024.100126","url":null,"abstract":"<div><p>For the first time, we present targeted protein detection by tryptic digestion of human chorionic gonadotropin (hCG) followed by electromembrane extraction (EME). Operational parameters were optimized, and urine and serum samples spiked with hCG underwent tryptic digestion followed by EME of the βT5 signature peptide. The liquid membrane comprised nitrophenyl octyl ether (NPOE), carvacrol, and di(2-ethyl hexyl) phosphate (DEHP) at ratios of 49:49:2 (w/w/w). Extractions were performed in a conductive vial format for 45 min at 5 V. Even from highly complex digested samples of serum and urine, the signature peptide βT5 was extracted by EME and detected by LC-MS/MS. While attempts to extract intact hCG protein were unsuccessful, the extraction of the signature peptide was efficient. The extraction recovery from undigested and digested urine was 71 % (RSD = 17 %) and 116 % (RSD = 17 %), respectively. For serum, the extraction recoveries were 11 % (RSD = 23 %) for undigested samples and 110 % (RSD = 14 %) for digested samples. This study demonstrates both the potential and challenges of EME for protein analysis. Experiments regarding EME of intact proteins provided new insights into protein phase distribution. This fundamental case study underscores the potential of EME as a sample preparation technique for the targeted determination of protein biomarkers and drugs.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"11 ","pages":"Article 100126"},"PeriodicalIF":5.2,"publicationDate":"2024-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582024000251/pdfft?md5=b5ab3fc079fe6bd42cb4a7567e4db57e&pid=1-s2.0-S2772582024000251-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142049377","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}