Analysis of biological samples containing synthetic cathinones has become a significant area of interest for researchers in recent years, because synthetic cathinones can cause adverse reactions such as delusions and hallucinations. Generally, the intricate nature of the sample matrix and exceedingly low drug concentration in biological samples present significant challenges for the determination of target substances. Accordingly, scientists were dedicated to the advancement of effective sample preparation techniques to address these difficulties. However, the current reviews involved in synthetic cathinones all focused on detection methods. A systematic review focusing on sample preparation for the quantification of synthetic cathinones is still lacking. In light of that, this paper reviewed the most commonly used sample preparation techniques for synthetic cathinones. Recent advances in sample preparation techniques for synthetic cathinones in different biological samples such as blood, urine, oral fluid and hair samples were discussed. In addition, we prospected the challenges and the future perspectives of biological sample preparation techniques for synthetic cathinones determination.
{"title":"Extraction of synthetic cathinones from biological samples: A systematic review","authors":"Mengjie Gu, Shutong Xue, Menghan Hou, Xiantao Shen","doi":"10.1016/j.sampre.2024.100133","DOIUrl":"10.1016/j.sampre.2024.100133","url":null,"abstract":"<div><div>Analysis of biological samples containing synthetic cathinones has become a significant area of interest for researchers in recent years, because synthetic cathinones can cause adverse reactions such as delusions and hallucinations. Generally, the intricate nature of the sample matrix and exceedingly low drug concentration in biological samples present significant challenges for the determination of target substances. Accordingly, scientists were dedicated to the advancement of effective sample preparation techniques to address these difficulties. However, the current reviews involved in synthetic cathinones all focused on detection methods. A systematic review focusing on sample preparation for the quantification of synthetic cathinones is still lacking. In light of that, this paper reviewed the most commonly used sample preparation techniques for synthetic cathinones. Recent advances in sample preparation techniques for synthetic cathinones in different biological samples such as blood, urine, oral fluid and hair samples were discussed. In addition, we prospected the challenges and the future perspectives of biological sample preparation techniques for synthetic cathinones determination.</div></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"12 ","pages":"Article 100133"},"PeriodicalIF":5.2,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142527745","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}
Pub Date : 2024-10-01DOI: 10.1016/j.sampre.2024.100134
Rafael O. Martins, Fernando M. Lanças
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 24–1 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 > 0.9900), with low limits of detection (LOD) and quantification (LOQ) ranging from 0.020 to 0.045 µg l-1 and 0.045 to 1.0 µg l-1 for pesticides, respectively, and 5 to 15 µg l-1 and 15 to 20 µg l-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.
{"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, 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<sup>4–1</sup> and 2<sup>3</sup> 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 > 0.9900), with low limits of detection (LOD) and quantification (LOQ) ranging from 0.020 to 0.045 µg <span>l</span><sup>-1</sup> and 0.045 to 1.0 µg <span>l</span><sup>-1</sup> for pesticides, respectively, and 5 to 15 µg <span>l</span><sup>-1</sup> and 15 to 20 µg <span>l</span><sup>-1</sup> 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}
Pub Date : 2024-10-01DOI: 10.1016/j.sampre.2024.100132
Irene Rodríguez-de Cos , Raibel Núñez-González , Rayco Guedes-Alonso , Sarah Piaugeard , María Esther Torres-Padrón , José Juan Castro-Hernández , Zoraida Sosa-Ferrera , José Juan Santana-Rodríguez
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 (Arbacia lixula, Paracentrotus lividus, Sphaerechinus granularis) 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.
{"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 , Raibel Núñez-González , Rayco Guedes-Alonso , Sarah Piaugeard , María Esther Torres-Padrón , José Juan Castro-Hernández , Zoraida Sosa-Ferrera , 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<sup>-1</sup> 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}
Pub Date : 2024-09-21DOI: 10.1016/j.sampre.2024.100131
Ester Hernández-Corroto , María Luisa Marina , María Concepción García
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.
{"title":"Simultaneous and sequential combination of techniques for the sustainable and extensive extraction of proteins and polyphenols from malt rootlets","authors":"Ester Hernández-Corroto , María Luisa Marina , 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}
Pub Date : 2024-09-14DOI: 10.1016/j.sampre.2024.100129
Petra Bianchini, Francesca Merlo, Valentina Quarta, Luca Ferrari, Chiara Milanese, Antonella Profumo, Andrea Speltini
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 %, n=3). 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.
{"title":"Improving sample preparation by biochar-coated sampling tubes: proof-of-concept extraction of sex hormones from real waters","authors":"Petra Bianchini, Francesca Merlo, Valentina Quarta, Luca Ferrari, Chiara Milanese, Antonella Profumo, 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<sup>−1</sup> 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}
Pub Date : 2024-09-12DOI: 10.1016/j.sampre.2024.100128
Laura Carbonell-Rozas, Roberto Romero-González, Antonia Garrido Frenich
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 (Camellia sinensis). 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.
{"title":"Green and miniaturized ultrasonic-assisted extraction using natural deep eutectic solvents to extract phenolic compounds from tea samples","authors":"Laura Carbonell-Rozas, Roberto Romero-González, 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<sup>−1</sup>. 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}
Pub Date : 2024-08-01DOI: 10.1016/j.sampre.2024.100125
Muhandiramge Ranasinghe, Michael C. Breadmore, Fernando Maya
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 >20 and extraction recoveries >70 % were achieved for nanoplastics concentrated at 500 V during 5 min. The limit of detection (LOD, S/N = 3) and limit of quantification (LOQ, S/N = 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 (n = 6) and interday (n = 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 (n = 3), with complete sample matrix removal of UV absorbing compounds.
{"title":"Preconcentration of nanoplastics using micro-electromembrane extraction across free liquid membranes","authors":"Muhandiramge Ranasinghe, Michael C. Breadmore, 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 >20 and extraction recoveries >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<sup>−4</sup>% (w/v) and 2.00×10<sup>−3</sup>% (w/v), respectively. Intraday (<em>n</em> = 6) and interday (<em>n</em> = 6) repeatability%RSD for 5.5 × 10<sup>−3</sup>% (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}
Pub Date : 2024-08-01DOI: 10.1016/j.sampre.2024.100126
Torstein Kige Rye , Frederik André Hansen , Trine Grønhaug Halvorsen , Stig Pedersen-Bjergaard
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.
{"title":"Electromembrane extraction of human chorionic gonadotropin – A case study on mass transfer of intact protein versus signature peptide","authors":"Torstein Kige Rye , Frederik André Hansen , Trine Grønhaug Halvorsen , 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}
Pub Date : 2024-08-01DOI: 10.1016/j.sampre.2024.100124
Donatella Ferrara , Marco Beccaria , Chiara E. Cordero , Giorgia Purcaro
Analyzing fatty acids provides key insights into fat composition for industrial applications and their implications for nutrition and health. Typically, fatty acid analysis involves extracting lipids from the matrix and converting them into fatty acid methyl esters (FAME) through a derivatization process before gas chromatography (GC) analysis. Either one-step or two-step procedures can be found in the literature and as official methods. In this work, different methods exploiting microwave-assisted processes were compared with two official methods from the American Oil Chemical Society (AOCS). Especially, two types of microwave-assisted extractions were employed: solvent extraction and extraction with hydrolysis. The extracts were derivatized using either BF3 or a microwave-assisted methanolic hydrogen chloride solution. These combinations of extraction and derivatization methods were compared also with one-step microwave-assisted extraction and derivatization, and two AOCS reference methods, resulting in seven different methods applied to six different food matrices. The performance of the different procedures was compared based on the FAME profile obtained from the comprehensive two-dimensional GC (GC × GC)-FID analysis.
Microwave-assisted processes were shown to be effective, yielding results comparable to the official methods in both the one-step and two-step methods. Moreover, it was shown that the BF3 derivatization could be safely replaced with microwave-assisted derivatization with methanolic hydrogen chloride, providing equivalent performances while enhancing operator safety and environmental friendliness. Some discrepancies in the FAMEs profile were highlighted for the sample of oats, the only explicitly requiring acidic hydrolysis for lipid extraction. Further studies are required to understand the reasons behind these differences and develop a suitable modified method. In conclusion, all the methods were evaluated for greenness and blueness with two specific tools: AGREEprep and BAGI.
{"title":"Comprehensive comparison of fatty acid methyl ester profile in different food matrices using microwave-assisted extraction and derivatization methods and comprehensive two-dimensional gas chromatography coupled with flame ionization detection","authors":"Donatella Ferrara , Marco Beccaria , Chiara E. Cordero , Giorgia Purcaro","doi":"10.1016/j.sampre.2024.100124","DOIUrl":"10.1016/j.sampre.2024.100124","url":null,"abstract":"<div><p>Analyzing fatty acids provides key insights into fat composition for industrial applications and their implications for nutrition and health. Typically, fatty acid analysis involves extracting lipids from the matrix and converting them into fatty acid methyl esters (FAME) through a derivatization process before gas chromatography (GC) analysis. Either one-step or two-step procedures can be found in the literature and as official methods. In this work, different methods exploiting microwave-assisted processes were compared with two official methods from the American Oil Chemical Society (AOCS). Especially, two types of microwave-assisted extractions were employed: solvent extraction and extraction with hydrolysis. The extracts were derivatized using either BF<sub>3</sub> or a microwave-assisted methanolic hydrogen chloride solution. These combinations of extraction and derivatization methods were compared also with one-step microwave-assisted extraction and derivatization, and two AOCS reference methods, resulting in seven different methods applied to six different food matrices. The performance of the different procedures was compared based on the FAME profile obtained from the comprehensive two-dimensional GC (GC × GC)-FID analysis.</p><p>Microwave-assisted processes were shown to be effective, yielding results comparable to the official methods in both the one-step and two-step methods. Moreover, it was shown that the BF<sub>3</sub> derivatization could be safely replaced with microwave-assisted derivatization with methanolic hydrogen chloride, providing equivalent performances while enhancing operator safety and environmental friendliness. Some discrepancies in the FAMEs profile were highlighted for the sample of oats, the only explicitly requiring acidic hydrolysis for lipid extraction. Further studies are required to understand the reasons behind these differences and develop a suitable modified method. In conclusion, all the methods were evaluated for greenness and blueness with two specific tools: AGREEprep and BAGI.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"11 ","pages":"Article 100124"},"PeriodicalIF":5.2,"publicationDate":"2024-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582024000238/pdfft?md5=7d9305659edce576aeacf487b7310e8c&pid=1-s2.0-S2772582024000238-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142058063","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}
Vacuum-assisted headspace solid-phase microextraction (Vac-HS-SPME) could provide an alternative for extracting pesticides from grape samples. Vac-HS-SPME method is utilized to the simultaneous analysis of six pesticides from various classes, namely boscalid, quizalofop-p-methyl, oxyfluorfen, fluroxypyr-meptyl, metribuzin and epoxiconazole. In this study investigated and optimized the impact of independent variables, such as extraction temperature, extraction time, fiber coating, incubation time, salt effect, sample volume, air evacuation time, pH, desorption time with the objective of achieving lower detection limits (ranging from 0.11 to 0.61 µg mL-1) and effective analyte responses. Moreover, in this work a comparison was made between classical solid phase microextraction and vacuum-assisted solid phase microextraction for the extraction of pesticides in grape samples under the same parameters. The results clearly demonstrated that the combination of Vac-HS-SPME proved to be more appropriate and selective for the extraction of pesticides from grape samples.
{"title":"Vacuum-assisted headspace-solid phase microextraction of pesticides in grape samples","authors":"Yerkanat Syrgabek, Mereke Alimzhanova, Saltanat Yegemova, Svetlana Batyrbekova","doi":"10.1016/j.sampre.2024.100123","DOIUrl":"https://doi.org/10.1016/j.sampre.2024.100123","url":null,"abstract":"<div><p>Vacuum-assisted headspace solid-phase microextraction (Vac-HS-SPME) could provide an alternative for extracting pesticides from grape samples. Vac-HS-SPME method is utilized to the simultaneous analysis of six pesticides from various classes, namely boscalid, quizalofop-p-methyl, oxyfluorfen, fluroxypyr-meptyl, metribuzin and epoxiconazole. In this study investigated and optimized the impact of independent variables, such as extraction temperature, extraction time, fiber coating, incubation time, salt effect, sample volume, air evacuation time, pH, desorption time with the objective of achieving lower detection limits (ranging from 0.11 to 0.61 µg mL<sup>-1</sup>) and effective analyte responses. Moreover, in this work a comparison was made between classical solid phase microextraction and vacuum-assisted solid phase microextraction for the extraction of pesticides in grape samples under the same parameters. The results clearly demonstrated that the combination of Vac-HS-SPME proved to be more appropriate and selective for the extraction of pesticides from grape samples.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"11 ","pages":"Article 100123"},"PeriodicalIF":5.2,"publicationDate":"2024-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582024000226/pdfft?md5=3796d3993afa256137a9e584dd76c6e9&pid=1-s2.0-S2772582024000226-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141596670","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}
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