Advances in Sample Preparation最新文献

{"title":"Microextraction by packed sorbent: Introducing a novel hybrid silica-based chitosan-graphene oxide biosorbent for the evaluation of pesticides and antibiotics in food matrices","authors":"Rafael O. Martins,&nbsp;Fernando M. Lanças","doi":"10.1016/j.sampre.2024.100134","DOIUrl":"10.1016/j.sampre.2024.100134","url":null,"abstract":"<div><div>This study introduces a novel silica-graphene oxide@chitosan (SiGO@CS) material as a packed biosorbent for microextraction by packed sorbent (MEPS), followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis of pesticides (atrazine and thiamethoxam) and antibiotics (ceftiofur and sulfonamide) in food samples. The graphene-based aerogel was modified with varying percentages of silica-graphene oxide/chitosan (w/w) and characterized to confirm successful chitosan incorporation. Optimization of the MEPS protocol, using 2^4–1 and 2³ experimental designs, identified draw/eject and washing cycles as the most influential parameters for extraction efficiency. The SiGO@CS biosorbent with 80 % CS/SiGO (w/w) exhibited superior extraction efficiency compared to other ratios and commercial sorbents. The method demonstrated excellent linearity for all analytes (R² &gt; 0.9900), with low limits of detection (LOD) and quantification (LOQ) ranging from 0.020 to 0.045 µg <span>l</span>^-1 and 0.045 to 1.0 µg <span>l</span>^-1 for pesticides, respectively, and 5 to 15 µg <span>l</span>^-1 and 15 to 20 µg <span>l</span>^-1 for antibiotics, respectively. Trueness values were within 82 % to 109 %. The method's green credentials were confirmed using AGREEprep and the Green Analytical Procedure Index (GAPI) approach, highlighting sorbent reusability (over 15 times) and rapid analytical throughput (5 min per sample) with low use of pre-treated sample extract volume (500 µL). The application to local corn, tomato, and milk samples confirmed the detection and quantification of thiamethoxam and atrazine at concentrations above the recommended ingestion per day for one sample of tomato and corn out of the three samples analyzed. Furthermore, using the novel SiGO@CS biosorbent in the MEPS protocol offers a green, high-performance analytical alternative to traditional sorbent phases, with the potential for evaluating trace levels of pesticides and antibiotics in food matrices.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"12 ","pages":"Article 100134"},"PeriodicalIF":5.2,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142593277","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":"A miniaturized QuEChERS-DLLME method for simultaneous determination of acetamide, acrylamide, and glycidamide in infant formula using GC–MS","authors":"J.A. Custodio-Mendoza ,&nbsp;M.P. España Fariñas ,&nbsp;A.M. Ares-Fuentes ,&nbsp;M.A. Kurek ,&nbsp;A.M. Carro Díaz","doi":"10.1016/j.sampre.2024.100141","DOIUrl":"10.1016/j.sampre.2024.100141","url":null,"abstract":"<div><div>Infant formula is the only food product suitable for infants during the first months of life. Therefore, evaluating food contaminants is essential for ensuring infant food safety. We developed a miniaturized QuEChERS (µ-QuEChERS) method combined with Dispersive Liquid-Liquid Microextraction (DLLME) to detect acrylamide, glycidamide, and acetamide in IF simultaneously. Several parameters were optimized, including sample size, extraction solvent, clean-up sorbent type, and amount, among others, using an asymmetrical factorial design. The method also incorporated xanthydrol derivatization under light-protected, acidic conditions within the DLLME process, improving selectivity and enrichment.</div><div>The µ-QuEChERS-DLLME method was validated according to FDA guidelines, demonstrating high selectivity, specificity, and excellent linearity (<em>r</em>² ≥ 0.9995). Recovery rates ranged from 91.0 % to 110.1 %, with precision (RSD ≤ 9.1 %). The method's sustainability was evaluated using the AGREEprep tool. It was applied to analyze acrylamide, glycidamide, and acetamide in 8 infant formula samples. Acetamide was quantifiable in one sample (230 ng/g), while acrylamide levels ranged from below the quantification limit to 50 ng/g, consistent with previous studies. This demonstrates the method's robustness for amide analysis in infant formula.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"12 ","pages":"Article 100141"},"PeriodicalIF":5.2,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142721808","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":"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":"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":"2024-10-01","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":"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":"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":"2024-10-01","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":"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":"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":"The determination of estrogens in fish samples by magnetic solid phase extraction coupled to high performance liquid chromatography-diode array detector","authors":"Bin Xue ,&nbsp;Mingzhong Xu ,&nbsp;Zuhai Bai ,&nbsp;Cong Hu","doi":"10.1016/j.sampre.2024.100120","DOIUrl":"https://doi.org/10.1016/j.sampre.2024.100120","url":null,"abstract":"<div><p>In this work, a novel magnetic nanoparticle (Fe₃O₄@SiO₂@MIL-53(Al)-NH₂) constructed on the basis of metal-organic frameworks (MOFs, MIL-53(Al)-NH₂) was prepared, which was characterized by Fourier transform infrared spectroscopy (FT-IR), transmission electron microscope (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). Good preparation reproducibility was obtained with the relative standard deviations (RSDs) ranging from 6.6 to 13.1 % (<em>n</em> = 6). In addition, the prepared Fe₃O₄@SiO₂@MIL-53(Al)-NH₂ possesses many merits, including simple preparation, greenness, good water/solvent stability and high specific surface area. The Fe₃O₄@SiO₂@MIL-53(Al)-NH₂ was used as an adsorbent for magnetic solid phase extraction (MSPE) of estrogens in fish samples. To achieve higher extraction efficiency, several factors including extraction time, pH value, ionic strength and desorption time were explored. Compared with other methods, the developed method exhibits high extraction efficiency, fast extraction kinetics and suitable for simultaneous analysis of large number of samples. The method was successfully applied to the analysis of estrogens in (spiked) fish samples, and good recoveries were obtained.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"11 ","pages":"Article 100120"},"PeriodicalIF":5.2,"publicationDate":"2024-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582024000196/pdfft?md5=018e2f4659ca4b8f2c415b3249eed798&pid=1-s2.0-S2772582024000196-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141479959","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}