Advances in Sample Preparation最新文献

Polydopamine-graphene oxide aerogel for in-tube solid-phase microextraction of polycyclic aromatic hydrocarbons

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2024.100144

Ziyi Jiang, Yanan Bu, Juanjuan Feng, Min Sun

Due to the wide distribution and potential carcinogenicity, teratogenicity and mutagenicity, polycyclic aromatic hydrocarbons (PAHs) have attracted much attention, requiring efficient and sensitive methods for detection. In order to improve the stability and extraction performance of graphene oxide aerogel, polydopamine was introduced to functionalize it. Polydopamine-hybridized graphene oxide aerogel was in-situ fabricated on the surface of titanium wire. The composite material was characterized by SEM and FT-IR. Three aerogel-coated wires were filled in a polyetheretherketone tube for in-tube solid-phase microextraction. Coupled with high performance liquid chromatography, the tube showed good extraction performance for several PAHs. Under the optimal conditions (sampling volume of 60 mL, sampling rate of 1.50 mL/min, sample pH of 7.3, 0.5 % (v/v) of methanol and 1.0 % (w/v) of NaCl in sample, desorption time of 1.0 min), an online analytical method was developed for determining trace PAHs from water samples, with low detection limits (0.01–0.05 μg/L), wide linear ranges (0.03–50 μg/L, 0.15–100 μg/L) with correlation coefficients (0.9953–0.9992) and satisfactory repeatability (RSDs, 0.22 %-4.42 % for intra-day, 1.42 %-5.18 % for inter-day). The method was applied to analyze some water samples including leaching solutions of coal ash and paper food box, some targets were found. The recoveries in these samples with different spiked levels (2.0 and 10.0 μg/L) were in the range of 81–117 %.

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引用次数: 0

Nitrogen-rich covalent organic polymers for efficient solid phase extraction of nonsteroidal anti-inflammatory drugs from water samples

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100148

Yuqi Cheng , Jia Li , Xiaochen Xiu , Xinghua Teng , Wen Zhang , Lei Ji , Leilei Wang

Non-steroidal anti-inflammatory drugs (NSAIDs) have received increasing attention owing to their ubiquitous occurrence in environmental water systems and adverse effects. In order to monitor trace levels of NSAIDs from complex water samples, development of facile and efficient sample pretreatment is of great significance. Herein, a nitrogen-rich covalent organic polymer containing phenyl, triazine and amine groups was fabricated via solvent-free copolymerization. Then, utilizing nitrogen-rich covalent organic polymer as adsorbent for solid phase extraction cartridges, the pretreatment method was combined with high-performance liquid chromatography-diode array detection to quantify five representative NSAIDs (ketoprofen, carprofen, flurbiprofen, diclofenac and mefenamic acid) in environmental water samples. Under the optimal extraction conditions (adsorbent amount: 40 mg; NaCl concentration: 0%; pH 6; extraction time: 20min; eluent solvent: 4 mL of formic acid/acetonitrile (5%, v/v)), the proposed method provided low detection limits (0.06–0.2 μg L^-1), wide linear ranges (0.2–100 μg L^-1) with correlation coefficients (0.9991–0.9997) and acceptable precision (RSDs, 6.6–8.5% for intra-day, 7.2–9.5% for inter-day). The practical application of the method was confirmed through the successful determination of NSAIDs in tap water, surface water, and sewage. The recoveries in these samples at the four NSAIDs concentration levels ranged from 81.3% to 109.8%, with the RSDs lower than 7.8%.

{"title":"Nitrogen-rich covalent organic polymers for efficient solid phase extraction of nonsteroidal anti-inflammatory drugs from water samples","authors":"Yuqi Cheng , Jia Li , Xiaochen Xiu , Xinghua Teng , Wen Zhang , Lei Ji , Leilei Wang","doi":"10.1016/j.sampre.2025.100148","DOIUrl":"10.1016/j.sampre.2025.100148","url":null,"abstract":"<div><div>Non-steroidal anti-inflammatory drugs (NSAIDs) have received increasing attention owing to their ubiquitous occurrence in environmental water systems and adverse effects. In order to monitor trace levels of NSAIDs from complex water samples, development of facile and efficient sample pretreatment is of great significance. Herein, a nitrogen-rich covalent organic polymer containing phenyl, triazine and amine groups was fabricated via solvent-free copolymerization. Then, utilizing nitrogen-rich covalent organic polymer as adsorbent for solid phase extraction cartridges, the pretreatment method was combined with high-performance liquid chromatography-diode array detection to quantify five representative NSAIDs (ketoprofen, carprofen, flurbiprofen, diclofenac and mefenamic acid) in environmental water samples. Under the optimal extraction conditions (adsorbent amount: 40 mg; NaCl concentration: 0%; pH 6; extraction time: 20min; eluent solvent: 4 mL of formic acid/acetonitrile (5%, v/v)), the proposed method provided low detection limits (0.06–0.2 μg L<sup>-1</sup>), wide linear ranges (0.2–100 μg L<sup>-1</sup>) with correlation coefficients (0.9991–0.9997) and acceptable precision (RSDs, 6.6–8.5% for intra-day, 7.2–9.5% for inter-day). The practical application of the method was confirmed through the successful determination of NSAIDs in tap water, surface water, and sewage. The recoveries in these samples at the four NSAIDs concentration levels ranged from 81.3% to 109.8%, with the RSDs lower than 7.8%.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"13 ","pages":"Article 100148"},"PeriodicalIF":5.2,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143130412","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}

引用次数: 0

Determination of acylcarnitines in intact brain tumors using coated blade spray mass spectrometry (CBS-MS)

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2024.100146

Joanna Bogusiewicz , Karol Jaroch , Jacek Furtak , Marcin Birski , Krystyna Soszyńska , Anna Majdańska , Agata Ryfa , Marek Harat , Barbara Bojko

Potential biomarkers of cancerous alterations could be selected by profiling a wide range of analytes. For this purpose, analytical platforms enabling detailed analysis of different biological matrices are applied. However, after biomarker selection, it is essential to shorten the analysis time as much as possible to speed up the diagnostic process. Therefore, this study aimed to optimize and test the coated blade spray mass spectrometry (CBS-MS) method in analyzing potential biomarkers in brain tumor studies: acylcarnitine. Meningiomas with different mutation statuses in NF2 were studied due to the relation of NF2 mutation with the higher risk of malignant transformation and multiple meningiomas. The application of CBS-MS enabled the determination of acetylcarnitine concentration (AC C2:0) and propionylcarnitine (AC C3:0) in intact tumor tissue. However, it would be necessary to enlarge the study group to confirm the conclusions on the concentration of these analytes in NF2 mutant and wild-type meningiomas. Apart from qualitative analysis, the simultaneous detection of a wide range of acylcarnitines in untargeted analysis was also possible.

{"title":"Determination of acylcarnitines in intact brain tumors using coated blade spray mass spectrometry (CBS-MS)","authors":"Joanna Bogusiewicz , Karol Jaroch , Jacek Furtak , Marcin Birski , Krystyna Soszyńska , Anna Majdańska , Agata Ryfa , Marek Harat , Barbara Bojko","doi":"10.1016/j.sampre.2024.100146","DOIUrl":"10.1016/j.sampre.2024.100146","url":null,"abstract":"<div><div>Potential biomarkers of cancerous alterations could be selected by profiling a wide range of analytes. For this purpose, analytical platforms enabling detailed analysis of different biological matrices are applied. However, after biomarker selection, it is essential to shorten the analysis time as much as possible to speed up the diagnostic process. Therefore, this study aimed to optimize and test the coated blade spray mass spectrometry (CBS-MS) method in analyzing potential biomarkers in brain tumor studies: acylcarnitine. Meningiomas with different mutation statuses in NF2 were studied due to the relation of NF2 mutation with the higher risk of malignant transformation and multiple meningiomas. The application of CBS-MS enabled the determination of acetylcarnitine concentration (AC C2:0) and propionylcarnitine (AC C3:0) in intact tumor tissue. However, it would be necessary to enlarge the study group to confirm the conclusions on the concentration of these analytes in NF2 mutant and wild-type meningiomas. Apart from qualitative analysis, the simultaneous detection of a wide range of acylcarnitines in untargeted analysis was also possible.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"13 ","pages":"Article 100146"},"PeriodicalIF":5.2,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143130329","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}

引用次数: 0

Maximizing the neuroprotection from Citrus aurantium leaves: Optimization of a blended extract from a sequential extraction process with compressed fluids and NADES

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100149

Victor M. Amador-Luna, Miguel Herrero, Marta Jiménez de la Parra, Ángel Gómez Arribas, Elena Ibáñez, Lidia Montero

Citrus aurantium, also known as bitter orange, and the by-products obtained during its processing are a rich source of bioactive compounds. In particular, leaves from the tree pruning and from fruits harvesting are considered an agrifood-related waste with high valorization potential. Considering the wide variety of bioactive compounds present in the leaves (carotenoids, terpenes and phenolic compounds), this study is focused on the valorization of C. aurantium pruning waste through a sequential three-step extraction process using green extraction techniques, i.e. supercritical fluid extraction (SFE), followed by pressurized liquid extraction (PLE) using natural deep eutectic solvents (NADES), and an antisolvent extraction to recover the remaining bioactive compounds adsorbed to the NADES and extraction residues. In this sense, this is the first time that PLE using NADES followed by an antisolvent step to re-extract the compounds from the PLE residue is presented. Moreover, different protocols to efficiently remove the NADES from the PLE extract were also studied for the first time. Due to the different nature and bioactivity of the obtained extracts, the mixture of the three fractions was optimized to enhance its overall preventive potential against neurodegenerative diseases. Finally, its scalability to a semi-pilot scale was evaluated, giving rise to increased bioactive values of the blended extract.

{"title":"Maximizing the neuroprotection from Citrus aurantium leaves: Optimization of a blended extract from a sequential extraction process with compressed fluids and NADES","authors":"Victor M. Amador-Luna, Miguel Herrero, Marta Jiménez de la Parra, Ángel Gómez Arribas, Elena Ibáñez, Lidia Montero","doi":"10.1016/j.sampre.2025.100149","DOIUrl":"10.1016/j.sampre.2025.100149","url":null,"abstract":"<div><div><em>Citrus aurantium</em>, also known as bitter orange, and the by-products obtained during its processing are a rich source of bioactive compounds. In particular, leaves from the tree pruning and from fruits harvesting are considered an agrifood-related waste with high valorization potential. Considering the wide variety of bioactive compounds present in the leaves (carotenoids, terpenes and phenolic compounds), this study is focused on the valorization of <em>C. aurantium</em> pruning waste through a sequential three-step extraction process using green extraction techniques, i.e. supercritical fluid extraction (SFE), followed by pressurized liquid extraction (PLE) using natural deep eutectic solvents (NADES), and an antisolvent extraction to recover the remaining bioactive compounds adsorbed to the NADES and extraction residues. In this sense, this is the first time that PLE using NADES followed by an antisolvent step to re-extract the compounds from the PLE residue is presented. Moreover, different protocols to efficiently remove the NADES from the PLE extract were also studied for the first time. Due to the different nature and bioactivity of the obtained extracts, the mixture of the three fractions was optimized to enhance its overall preventive potential against neurodegenerative diseases. Finally, its scalability to a semi-pilot scale was evaluated, giving rise to increased bioactive values of the blended extract.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"13 ","pages":"Article 100149"},"PeriodicalIF":5.2,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143131052","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}

引用次数: 0

DES modified silica gel as dispersing material for miniaturized matrix solid phase dispersion applied to triazoles determination

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100153

Susanna Della Posta , Valeria Gallo , Emanuele Limiti , Marcella Trombetta , Monica Gherardi , Alessandra Gentili , Laura De Gara , Chiara Fanali

Matrix solid phase dispersion (MSPD) represents one of the most useful methods for pesticides determination in vegetables. This extraction method involves the use of a solid, dispersing material, which is homogenized together with the sample in a mortar and loaded into a cartridge for the analyte's elution with a suitable solvent. Innovative MSPDs involve the use, as dispersing material, of silica gel (SCG) impregnated with deep eutectic solvents (DESs). SCG high porosity can facilitate DES impregnation process due to hydrogen bonds or electrostatic interactions among them.

A miniaturized MSPD extraction for triazoles from tomato using as dispersant DES modified SCG, followed by HPLC-MS extracts analysis, was developed. Four DES modified SCGs were tested in the MSPD procedure and the best result in terms of extracted triazoles was obtained using a choline chloride – Propylene Glycol DES modified SCG. Ethyl Acetate was selected as MSPD procedure extractive solvent resulting more efficient than methanol, acetonitrile and chloroform. The optimization of the extraction procedure involved the study of SCG to DES ratio (w/v), sample to dispersing material ratio (w/w) and extractive solvent volume able to obtain the greatest recovery of triazoles from tomato. The optimized method was validated and maximum values of 3.6 % and 8.3 % were obtained for intra-day and inter-day precision respectively. For each analyte the calculated limit of quantification was similar or lower than their Maximum Residue Limit. Triazoles mean recovery ranged from 70 to 102 %.

The new ChCl-propylene glycol DES modified SCG represents a valid alternative to conventional dispersing material in MSPD procedure apply to pesticides determination.

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引用次数: 0

Automated capillary electrophoresis analyses of dried blood samples after patient-centric volumetric absorptive microsampling

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2024.100142

Richard Maršala , Miloš Dvořák , Pavel Kubáň

An automated method for the analysis of dried blood samples collected by volumetric absorptive microsampling (VAMS) is presented for the first time. A single commercial capillary electrophoresis (CE) instrument (with no need for hardware or software modifications) was employed for the expeditious analyses of the dried material using several integral and novel features. These included the use of external pressure for sub-minute sample preparation from Mitra® VAMS polymeric tips, the use of the sampling tips as inherent micro-agitators for instant eluate homogenization, preparation/sampling at the CE outlet for more convenient capillary length adjustment, and short-end injection for sub-minute CE separation and quantification of lactate as a model analyte.

The operational parameters for the sample preparation and analysis were comprehensively evaluated resulting in a baseline separation of lactate from all endogenous matrix compounds. The optimized method demonstrated excellent intra- and inter-day repeatability of peak areas (RSD values ≤ 7.2 %), linearity (R² = 0.9990) over the clinically relevant concentration range (0.15 – 20 mM), the limits of detection and quantification at 0.03 and 0.1 mM, respectively, and a sample throughput ≥ 16 samples/hour. No ageing was observed for VAMS devices stored at ambient conditions for up to 14 days. Comparative analysis with a portable lactate analyser revealed slightly elevated concentrations in dried vs. liquid capillary blood due to the glycolysis of glucose during drying, nevertheless, lactate concentrations in Mitra® devices correlated well with those in blood plasma, which is typically used in clinical practice.

The present study offers a robust, accurate, and environmentally benign concept for the automated analyses of VAMS-collected blood samples with its potential application in patient-centric sampling, clinical diagnostics and research, and personalized healthcare.

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引用次数: 0

Advances in applications of metal-organic frameworks for selective solid-phase extraction and chromatographic separation of active pharmaceutical ingredients

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100151

Zhenyu Song , Bodong Liu , Zezhou Zang , Zeyi Li , Ying Jiang , Tiantian Si , Min Sun

Active pharmaceutical ingredients (APIs) constitute a fundamental component in the development and clinical application of pharmaceuticals, thereby playing an indispensable and pivotal role within the realm of biomedicine. In current research, metal-organic frameworks (MOFs) have garnered considerable attention for studying APIs, serving as effective adsorbents for the extraction of APIs or as stationary phases for their separation. Notably, MOFs composites have significantly enhanced the enrichment and selectivity for APIs by modifying their size, micropore structure, surface characteristics, and charge. The mechanisms underlying these improvements include hydrogen bonding, π-stacking interactions, electrostatic interactions, hydrophobic interactions, and hydrophilic interactions. This comprehensive review focuses on the latest advancements and breakthroughs in the application of MOFs for selective extraction, enrichment, and chromatographic separation of APIs within solid-phase extraction, solid-phase microextraction, and chromatographic stationary phases spanning the period from 2020 to 2024. Additionally, the review highlights the potential development of MOFs in sample preparation chromatographic separation for application, particularly for APIs derived from traditional Chinese medicine (TCM), providing valuable insights into the research and development of nanomaterials such as MOFs in using APIs.

{"title":"Advances in applications of metal-organic frameworks for selective solid-phase extraction and chromatographic separation of active pharmaceutical ingredients","authors":"Zhenyu Song , Bodong Liu , Zezhou Zang , Zeyi Li , Ying Jiang , Tiantian Si , Min Sun","doi":"10.1016/j.sampre.2025.100151","DOIUrl":"10.1016/j.sampre.2025.100151","url":null,"abstract":"<div><div>Active pharmaceutical ingredients (APIs) constitute a fundamental component in the development and clinical application of pharmaceuticals, thereby playing an indispensable and pivotal role within the realm of biomedicine. In current research, metal-organic frameworks (MOFs) have garnered considerable attention for studying APIs, serving as effective adsorbents for the extraction of APIs or as stationary phases for their separation. Notably, MOFs composites have significantly enhanced the enrichment and selectivity for APIs by modifying their size, micropore structure, surface characteristics, and charge. The mechanisms underlying these improvements include hydrogen bonding, π-stacking interactions, electrostatic interactions, hydrophobic interactions, and hydrophilic interactions. This comprehensive review focuses on the latest advancements and breakthroughs in the application of MOFs for selective extraction, enrichment, and chromatographic separation of APIs within solid-phase extraction, solid-phase microextraction, and chromatographic stationary phases spanning the period from 2020 to 2024. Additionally, the review highlights the potential development of MOFs in sample preparation chromatographic separation for application, particularly for APIs derived from traditional Chinese medicine (TCM), providing valuable insights into the research and development of nanomaterials such as MOFs in using APIs.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"13 ","pages":"Article 100151"},"PeriodicalIF":5.2,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143130413","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}

引用次数: 0

Greener and rapid magnetic solid phase microextraction method using Fe3O4@Al2O3/AC for chromatographic determination of neonicotinoid pesticides in vegetable oils

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100152

Musiiwa V. Sengane , Masixole Sihlahla , Philiswa N. Nomngongo , Nomvano Mketo

A greener sample preparation method based on magnetic solid phase microextraction (MSPμE) was developed for the preconcentration of neonicotinoid pesticides (acetamiprid, imidacloprid, thiacloprid and thiamethoxam) in vegetable oil samples followed by separation and quantification using high performance liquid chromatography with diode array detector (HPLC-DAD). Different characterisation techniques such as Fourier Transform Infrared Spectroscopy (FTIR), Powder X-ray diffraction analysis (PXRD), Thermogravimetric Analysis (TGA), Transmission electron microscopy (TEM), and scanning electron microscope and energy-dispersive X-ray spectroscopy (SEM-EDS) confirmed the synthesised magnetic nano adsorbents (Fe₃O₄, Fe₃O₄@Al₂O₃ and Fe₃O₄@Al₂O₃/AC). The most influential parameters affecting MSPμE of NEOs by Fe₃O₄@Al₂O₃/AC were examined using a multivariate optimisation approach and 8 min extraction time, 13 pH, 9 mg adsorbent mass, and 0.5 mL eluent volume were optimal parameters. The proposed Fe3O4@Al2O3/AC method showed high accuracy (80–119.21%) and precision (≤10 %) for all the investigated NEOs. Additionally, the obtained limit of detection (LOD) ranged from 0.5–1.76 ng µL^-1, the limit of quantification (LOQ) ranged from 1.87–6.62 ng µL^-1 and satisfactory high preconcentration factors (73.02- 407.0) were comparable with literature reported studies. The Analytical GREEness calculator AGREE, BAGI and NEMI analysis confirmed greenness of MSPμE. After that, the validated MSPμE method was applied to real vegetable oil samples (avocado, canola, olive and sunflower), and fortunately, all the investigated NEOs were below LODs of the proposed MSPμE /HPLC-DAD methods.

{"title":"Greener and rapid magnetic solid phase microextraction method using Fe3O4@Al2O3/AC for chromatographic determination of neonicotinoid pesticides in vegetable oils","authors":"Musiiwa V. Sengane , Masixole Sihlahla , Philiswa N. Nomngongo , Nomvano Mketo","doi":"10.1016/j.sampre.2025.100152","DOIUrl":"10.1016/j.sampre.2025.100152","url":null,"abstract":"<div><div>A greener sample preparation method based on magnetic solid phase microextraction (MSPμE) was developed for the preconcentration of neonicotinoid pesticides (acetamiprid, imidacloprid, thiacloprid and thiamethoxam) in vegetable oil samples followed by separation and quantification using high performance liquid chromatography with diode array detector (HPLC-DAD). Different characterisation techniques such as Fourier Transform Infrared Spectroscopy (FTIR), Powder X-ray diffraction analysis (PXRD), Thermogravimetric Analysis (TGA), Transmission electron microscopy (TEM), and scanning electron microscope and energy-dispersive X-ray spectroscopy (SEM-EDS) confirmed the synthesised magnetic nano adsorbents (Fe<sub>3</sub>O<sub>4</sub>, Fe<sub>3</sub>O<sub>4</sub>@Al<sub>2</sub>O<sub>3</sub> and Fe<sub>3</sub>O<sub>4</sub>@Al<sub>2</sub>O<sub>3</sub>/AC). The most influential parameters affecting MSPμE of NEOs by Fe<sub>3</sub>O<sub>4</sub>@Al<sub>2</sub>O<sub>3</sub>/AC were examined using a multivariate optimisation approach and 8 min extraction time, 13 pH, 9 mg adsorbent mass, and 0.5 mL eluent volume were optimal parameters. The proposed Fe3O4@Al2O3/AC method showed high accuracy (80–119.21%) and precision (≤10 %) for all the investigated NEOs. Additionally, the obtained limit of detection (LOD) ranged from 0.5–1.76 ng µL<sup>-1</sup>, the limit of quantification (LOQ) ranged from 1.87–6.62 ng µL<sup>-1</sup> and satisfactory high preconcentration factors (73.02- 407.0) were comparable with literature reported studies. The Analytical GREEness calculator AGREE, BAGI and NEMI analysis confirmed greenness of MSPμE. After that, the validated MSPμE method was applied to real vegetable oil samples (avocado, canola, olive and sunflower), and fortunately, all the investigated NEOs were below LODs of the proposed MSPμE /HPLC-DAD methods.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"13 ","pages":"Article 100152"},"PeriodicalIF":5.2,"publicationDate":"2025-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143131053","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}

引用次数: 0

Vial-coated thin film microextraction for perfluoroalkyl carboxylic acids (PFCAs) determination in water by GC–MS

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100147

J․Mabel Luna-Díaz , Luz O․ Leal-Quezada , Laura Ferrer , Edwin Palacio

Perfluoroalkyl carboxylic acids (PFCAs), a subclass of perfluoroalkyl substances (PFAs) commonly detected in water, are of increasing concern due to their persistence, bioaccumulative nature, and harmful effects on health. Determining PFCAs in environmental matrices is challenging because they are typically present at ng L⁻¹ levels and tend to adsorb onto materials like filtration membranes, causing significant losses during analysis. To address these challenges, a thin-film microextraction (TFME)-coated vial was designed for PFCA (C5–C10) extraction, coupled with gas chromatography-mass spectrometry (GC–MS). Glass was selected as the support material due to its low adsorption rate and superior chemical resistance compared to other polymers. The TFME coating, made from a weak anion exchange resin and polyacrylonitrile (10 % w/w) as a binder polymer, effectively extracts analytes from complex matrices while minimizing co-extraction of interfering macromolecules. The method eliminates the need for sample filtration, preventing PFCA loss in filtration membranes. Under optimal conditions, the extraction efficiency ranged from 70 to 100 %. Detection and quantification limits were 0.13–2.1 ng L⁻¹ and 0.42–7.1 ng L⁻¹, respectively. Intra- and inter-assay relative standard deviations (% RSD) were 4.9–2.2 % and 4.8–2.3 %, respectively, with a linear working range of 10–1000 ng L⁻¹ for the TFME-coated device. This method is suitable for PFCA determination in drinking water and complies with the Directive 2020/2184, which sets a maximum allowable limit of 500 ng L⁻¹ for total PFAs.

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引用次数: 0

Towards eco-metabolomics: NADES-guided extraction enables semi-quantitative metabolomics for Melissa officinalis

IF 5.2 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation

Pub Date : 2025-02-01 DOI: 10.1016/j.sampre.2025.100154

Chiara Spaggiari , Isa Sara Aimee Hiemstra , Antoinette Kazbar , Gabriele Costantino , Laura Righetti

In recent years, there has been a growing emphasis on the development of green extraction techniques that minimize environmental impact while maximizing yield of the extracted compounds. To this aim, in this study we investigated the potential of green solvents for extracting bioactive compounds from Melissa officinalis (MO) leaves. Specifically, we focus on the application of 20 Natural Deep Eutectic Solvents (NADES) with a relative polarity ranging from 0.34 to 1.29. Their extraction affinity against a set of 11 plant metabolites was predicted using COSMO-RS software and experimentally validated using quantitative LCHRMS analysis. Subsequently, the same extracts were subjected to non-target metabolomics to uncover the NADES selectivity towards the wide spectrum of MO leaf metabolites. Data preprocessing and feature alignment were performed using MZmine, and aligned features were annotated using SIRIUS+CSI:FingerID.

Overall, 249 and 195, metabolites were annotated in positive and negative ionization ion mode, respectively. Additionally, to have a more accurate view of the different NADES extraction capacity, we adopted a semi-quantitative approach that enables the prediction of concentration for all the annotated metabolites (N = 444).

The results highlighted the selectivity of some NADES in extracting very diverse biochemical classes, providing valuable insights into the composition and concentration of bioactive compounds. Interestingly, thymol-menthol NADES demonstrated the ability to efficiently extract a broad range of bioactive compounds, yielding a metabolome comparable to that obtained with conventional ethanolic. Overall, the entire workflow facilitated the green extraction and annotation of known bioactive molecules that had never been described in MO.

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引用次数: 0