{"title":"Monitoring the benefits of varying the template/monomer proportion in the synthesis of an ion-imprinted polymer for Ra(II) extraction","authors":"Marine Boudias , Alkiviadis Gourgiotis , Charlotte Cazala , Valérie Pichon , Nathalie Delaunay","doi":"10.1016/j.sampre.2022.100049","DOIUrl":"https://doi.org/10.1016/j.sampre.2022.100049","url":null,"abstract":"<div><p>In our previous paper, an ion-imprinted polymer (IIP) was for the first time synthesized for Ra(II) extraction using Ba(II) as template ion since it has properties close to Ra(II), acetonitrile/dimethylsulfoxide (1/1, v/v) as porogen, vinylphosphonic acid as complexing monomer, styrene as co-monomer, and divinylbenzene as cross-linker. The present study aims at investigating the influence of the template ion/monomer proportion (1/4, 1/6, and 1/8) on sorbents properties. Polymers were packed in solid phase extraction (SPE) cartridges for characterization. A particular attention was paid to control the impact of this ratio on the retention of Ra(II) and interfering ions (<em>i.e.</em> specificity) on IIPs, their capacity, and their breakthrough volume. Although the IIPs 1/4 and 1/8 tended to be slightly more specific than IIP 1/6, the adsorption capacity of the IIP 1/4 was much lower (0.3 µmol g<sup>−1</sup>) than the two others (3 µmol g<sup>−1</sup>). Data modelling indicated that Sips and Redlich-Peterson models were best fitted, sign of a monolayer adsorption process into cavities not completely homogeneous in contrast to the Langmuir model. IIPs 1/6 and 1/8 showed both high breakthrough volumes (>80 mL for 100 ng of Ba(II) percolated on 100 mg of sorbents) and BET experiments demonstrated no impact of the monomer proportion on surface area of the IIPs 1/4, 1/6, and 1/8. The repeatability of the synthesis was evaluated on the IIP 1/6. The SPE profiles resulting from three independent syntheses of the IIP 1/6 were very similar and thermogravimetric and BET analyses also confirmed that the three IIPs had similar physical characteristics. The IIP 1/6 was applied to the extraction of Ba(II) from spiked mineral waters (Mont Roucous® and Volvic®). The Ba(II) extraction recovery was subjected to matrix effects but those were solved by adapting the amount of sorbent to the volume of percolation solution. The optimized procedure has been successfully applied to extract <sup>226</sup>Ra for the first time with a dedicated IIP in a real sample: 5 mL of Mont Roucous® water were spiked with 80 mBq L<sup>−1</sup> of <sup>226</sup>Ra and <sup>228</sup>Ra which was used as tracer to perform quantification by isotope dilution. After extraction, the <sup>226</sup>Ra activity (88 ± 7 mBq L<sup>−1</sup>, coverage factor k = 2) and recovery on IIP 1/6 (93%) were determined using an Inductively Coupled Plasma Mass Spectrometer and the limit of quantification of the method was estimated at 19 mBq L<sup>−1</sup> (0.52 pg L<sup>−1</sup>).</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"5 ","pages":"Article 100049"},"PeriodicalIF":0.0,"publicationDate":"2023-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49752121","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Florencia Cora Jofre , Silvana M. Azcarate , José M. Camiña , Pablo Pacheco , Marianela Savio
{"title":"Assessing the greenness of optimized ultrasound and infrared assisted extraction through analytical metrics","authors":"Florencia Cora Jofre , Silvana M. Azcarate , José M. Camiña , Pablo Pacheco , Marianela Savio","doi":"10.1016/j.sampre.2023.100054","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100054","url":null,"abstract":"<div><p>Sample preparation involves a critical step due to the high organic matter content that implies its decomposition, prior to analysis. Two alternative analytical strategies for sample preparation employing diluted HNO<sub>3</sub> were optimized and compared, assisted by ultrasound (USAE) and infrared (IRAE) radiation. Multielement determination was achieved by MIP OES. For optimization of experimental conditions, a central composite design centered on the faces was carried out, considering four and five factors for IRAE and USAE, respectively. Dissolved organic carbon (DOC), residual acidity (RA) and solid residue (SR), significantly influence the responses to be evaluated. The response surface methodology was implemented to find the best combination of mass, diluted reagents (HNO<sub>3</sub> and H<sub>2</sub>O<sub>2</sub>), time and temperature in order to minimize responses for elemental extraction in animal feed samples. The optimized experimental conditions: 500 mg of sample mass, 60 °C of bath temperature, 30 min of extraction time, 2 mol L<sup>−1</sup> HNO<sub>3</sub> and 27% H<sub>2</sub>O<sub>2</sub>, were used to validate the USAE procedure. The conditions established for IRAE were 500 mg of the swine feed sample, followed by the addition of 2 mL of 2 mol L<sup>−1</sup> HNO<sub>3</sub> and 23% H<sub>2</sub>O<sub>2</sub>, irradiating for 23 min. Recoveries ranged from 81 to 114%, with good precision (RSD < 4%). Using five index tools the greenness of the proposed methods was demonstrated. According to IRAE simplicity, reliability, fast and easy to implement, it was successfully applied to the determination of Ca, Cu, Fe, K, Mg, Mn, P and Zn in agrifood samples.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"5 ","pages":"Article 100054"},"PeriodicalIF":0.0,"publicationDate":"2023-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49759085","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Marisol González-Bermúdez, Ángela I. López-Lorente, Rafael Lucena, Soledad Cárdenas
{"title":"Paper-based sorptive phases for a sustainable sample preparation","authors":"Marisol González-Bermúdez, Ángela I. López-Lorente, Rafael Lucena, Soledad Cárdenas","doi":"10.1016/j.sampre.2023.100051","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100051","url":null,"abstract":"<div><p>In recent years, using natural materials to prepare sorbents has been a clear trend in the sample preparation context. This research line is supported by sustainable considerations, as it responds to the tenth principle of Green Analytical Chemistry. Also, the affordability and availability of natural materials open the door to developing global analytical solutions. Among all the available natural materials, cellulose paper presents unique characteristics (porosity, mechanical resistance, and easy chemical/physical modification of the substrate) that can be exploited in analytical extractions. This article reviews the role of paper-based sorptive phases in the current sample preparation realm, putting more emphasis on their potential than on the description of specific applications. The article covers the main synthetic routes described in the literature for preparing these phases and the reported coatings. In contrast with the classical analytical workflow (based on the separated extraction, elution, and analysis steps), the direct combination of sample preparation with instrumental techniques permits further simplification of the analytical procedures. Cellulose paper can operate under both workflows, and the main approaches based on spectroscopic and spectrometric analysis will be discussed. Finally, the combination of both instrumental techniques (using the so-called dual substrates) will be outlined.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"5 ","pages":"Article 100051"},"PeriodicalIF":0.0,"publicationDate":"2023-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49752275","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Fabric phase sorptive extraction for environmental samples","authors":"Núria Fontanals, Francesc Borrull, Rosa M. Marcé","doi":"10.1016/j.sampre.2022.100050","DOIUrl":"https://doi.org/10.1016/j.sampre.2022.100050","url":null,"abstract":"<div><p>Fabric phase sorptive extraction (FPSE) has gradually become more widespread as a novel sorptive extraction technique since it has a number of advantages including a wide range of available materials, cheap and easy performance and highly efficient extraction. Because of this, FPSE has been applied in different fields to extract various types of analytes from different kinds of samples. In particular, it has been widely used in environmental applications.</p><p>This review covers the use of FPSE in environmental samples. It discusses the optimization of the variables involved during FPSE and presents novel FPSE approaches applied to environmental samples. It also reviews figures of merit obtained using the FPSE methods developed and summarizes data on the occurrence of contaminants in different types of environmental samples. This is done by looking at a selection of different studies in which FPSE is applied to analyze environmental samples.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"5 ","pages":"Article 100050"},"PeriodicalIF":0.0,"publicationDate":"2023-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49752122","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Waleed Alahmad , S. Irem Kaya , Ahmet Cetinkaya , Pakorn Varanusupakul , Sibel A. Ozkan
{"title":"Green chemistry methods for food analysis: Overview of sample preparation and determination","authors":"Waleed Alahmad , S. Irem Kaya , Ahmet Cetinkaya , Pakorn Varanusupakul , Sibel A. Ozkan","doi":"10.1016/j.sampre.2023.100053","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100053","url":null,"abstract":"<div><p>In recent years, food quality and safety have gained increasing attention. However, due to the complexity of food composition, accurate classical extraction techniques require using toxic organic solvents. The development of green extraction techniques has come to the fore to repress this drawback. In this review, the recent novel methodologies for extracting pollutants from food samples that fulfill the principles of green chemistry were summarized. The use of sorbent-based techniques, such as solid-phase microextraction (SPME), and stir-bar sorbent extraction (SBSE), and advanced techniques such as ultrasound-assisted extraction (UAE), microwave-assisted extraction (MAE), enzyme-assisted extraction (EAE), pressurized liquid extraction (PLE) and supercritical fluid extraction (SFE), for improving and accelerating extraction efficiency and reducing solvent consumption are highlighted. Lastly, future perspectives on the implementation of these eco-friendly methodologies are described along with the technological advancements required.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"5 ","pages":"Article 100053"},"PeriodicalIF":0.0,"publicationDate":"2023-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49727271","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Audrey Laberge-Carignan , Justine Basque , Emmanuel Tessier , Patrice Roberge , Jean Ruel , André Bégin-Drolet , Dominic Larivière
{"title":"New sample collection and dissolution tools for point-of-need analysis of Pb and Hg in fish tissues.","authors":"Audrey Laberge-Carignan , Justine Basque , Emmanuel Tessier , Patrice Roberge , Jean Ruel , André Bégin-Drolet , Dominic Larivière","doi":"10.1016/j.sampre.2022.100044","DOIUrl":"10.1016/j.sampre.2022.100044","url":null,"abstract":"<div><p>The quantification of contaminants in indigenous food is a significant consideration for food safety and security. This is particularly critical for remote communities that rely on local agriculture, fishing, and hunting as their primary food supply. While point-of-need technologies have been proposed to facilitate on-site detection and quantification of contaminants, sample preparation steps remain mandatory for most contaminants, especially inorganic ones. This study presents innovations to facilitate sample preparation at the point-of-need. First, the repeatability and reproducibility of two biopsy punch tools used to sample fish tissues (fillets) are assessed and compared. The first punch tool is commercially available (69039; Hatfield, PA) while the second was custom made. They were both simple to use and their results showed limited variability for mass collection. Second, a new, portable, low-energy-consumption ultrasonic probe for the rapid dissolution (< 10 min) of fish tissues in tetramethyl ammonium hydroxide (TMAH) is presented. The dissolution rate, and Hg and Pb recovery rates in fish tissues are also reported and compared to those obtained with an ultrasonic bath. Finally, the analytical performances of both tools were validated on certified reference materials for mercury after analysis by GC-ICP-MS. These new tools will improve chemical sampling success even for inexperienced users at the point-of-need.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"4 ","pages":"Article 100044"},"PeriodicalIF":0.0,"publicationDate":"2022-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582022000419/pdfft?md5=ae1e4d8380a5cd8a9d1550762dc35074&pid=1-s2.0-S2772582022000419-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87322139","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":"Preparation and further evaluation of l-menthol-based natural deep eutectic solvents as supported liquid membrane for the hollow fiber liquid-phase microextraction of sulfonamides from environmental waters","authors":"Myriam Díaz-Álvarez, Antonio Martín-Esteban","doi":"10.1016/j.sampre.2022.100047","DOIUrl":"10.1016/j.sampre.2022.100047","url":null,"abstract":"<div><p>In this work, the use of a hydrophobic natural deep eutectic solvent (NADES) as supported liquid membrane (SLM) for hollow fiber liquid-phase microextraction (HF-LPME) of sulfonamides is proposed. Different NADES based on <span>l</span>-menthol and naturally occurring organic acids (citric acid, formic acid, acetic acid, decanoic acid, nonanoic acid, lactic acid, valeric acid, isobutyric acid, hexanoic acid, octanoic acid, and 2-methylbutyric acid) were prepared at different molar ratios. Important solvent properties to work as SLM were studied such as stability in the fiber and compatibility with HPLC. Then, the ability of the prepared NADES to extract 8 antibiotics of the family of sulfonamides (SAs) from water by HF-LPME was studied. From them, the combination of formic acid:L-menthol (1:1) was selected as optimum since it provided a better and more balanced extraction of SAs. The optimized HF-LPME procedure was applied to the analysis of an artificial water containing humic acids, tap and river water samples, showing a good clean-up ability for all the tested samples. Calibration curves showed good linearity for all the SAs and samples with linear regression coefficients (r<sup>2</sup>) greater than 0.992. Relative recoveries ranged from 53 to 121%, with relative standard deviation values between 5 and 21%, depending upon the analyte and type of water sample. The limits of detection of the method varied from 0.63 to 2.85 µg/L for tap water, 0.70 to 3.23 µg/L for the Jarama river and 0.61 to 2.52 µg/L for the Manzanares river. Besides, the proposed method can be considered sustainable, according to AGREEprep tool, and greener than reported methods in the literature based in other microextraction techniques.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"4 ","pages":"Article 100047"},"PeriodicalIF":0.0,"publicationDate":"2022-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582022000444/pdfft?md5=dd1f0a98f3461f44e460e2a211eab835&pid=1-s2.0-S2772582022000444-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75974751","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}
Angelica Fina , Steven Mascrez , Marco Beccaria , Chiara De Luca , Juan Aspromonte , Chiara Cordero , Giorgia Purcaro
{"title":"A high throughput method for fatty acid profiling using simultaneous microwave-assisted extraction and derivatization followed by reversed fill/flush flow modulation comprehensive multidimensional gas chromatography","authors":"Angelica Fina , Steven Mascrez , Marco Beccaria , Chiara De Luca , Juan Aspromonte , Chiara Cordero , Giorgia Purcaro","doi":"10.1016/j.sampre.2022.100039","DOIUrl":"10.1016/j.sampre.2022.100039","url":null,"abstract":"<div><p>The fatty acid composition of a food product provides information regarding the origin of the product and its overall quality, such as its nutritional value. This work proposes a fast and accurate method for preparing fatty acid methyl esters from a wide variety of food products by using a single-step microwave-assisted extraction and derivatization coupled to reversed fill/flush flow modulation comprehensive two-dimensional gas chromatography (GC×GC) – flame ionization detector (FID) to tentatively identify and quantify the individual fatty acid. The robustness of the GC×GC – FID platform was successfully assessed, as well as the reliability of the entire proposed procedure, assuring repeatability largely below 10%. The enhanced separation obtained by the use of GC×GC allowed for the identification of 81 FAMEs in a single run of 30 min. The fatty acid methyl esters profiles obtained with the proposed microwave-assisted extraction and derivatization were comparable with reference methods from the literature and the American Oil Chemistry Society. This method also proved to be a significant step towards a greener procedure than the reference one when evaluated based on the PrepAGREE metrics that have been recently proposed.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"4 ","pages":"Article 100039"},"PeriodicalIF":0.0,"publicationDate":"2022-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582022000365/pdfft?md5=4160c29e760eed84d8fc4f2ba333e6f0&pid=1-s2.0-S2772582022000365-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88571527","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}
Inmaculada de la Calle, Diego Fernández-Rodríguez, Isela Lavilla, Carlos Bendicho
{"title":"Silver nanoparticle-cellulose composite for thin-film microextraction of Cd and Pb as dithiocarbamate derivatives followed by inductively-coupled plasma mass spectrometry determination","authors":"Inmaculada de la Calle, Diego Fernández-Rodríguez, Isela Lavilla, Carlos Bendicho","doi":"10.1016/j.sampre.2022.100041","DOIUrl":"10.1016/j.sampre.2022.100041","url":null,"abstract":"<div><p>Preconcentration of Cd and Pb at ultratrace level in waters following filtration through silver nanoparticles-cellulose composites used for thin-film microextraction was performed. The new procedure was based on the formation of pyrrolidine dithiocarbamate (APDC) derivatives, which showed a large affinity toward the AgNPs. For this purpose, cellulose filters modified with AgNPs were prepared <em>in situ</em> upon reduction of silver ions by sodium tetrahydroborate. The effect of several experimental parameters such as the kind of derivatization agent and its concentration, sample pH, desorption conditions and volume of filtered sample was assessed. Cd and Pb were quantitated in the eluates by inductively coupled plasma-mass spectrometry (ICP-MS). Filters were characterized by scanning electron microscopy (SEM) in backscattering electron mode and combined with energy dispersive X-ray spectrometry, showing the presence of Ag and S in the cellulose filter. The repeatability expressed as relative standard deviation (RSD,%) was 1.4% for Cd and 5.8% for Pb. Methodological detection limits were 0.6 and 8.5 ng/L for Cd and Pb, respectively. The method was applied to several environmental waters.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"4 ","pages":"Article 100041"},"PeriodicalIF":0.0,"publicationDate":"2022-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582022000389/pdfft?md5=5fba7b0774f1dec351f6af8249aa5f51&pid=1-s2.0-S2772582022000389-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78702120","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}
Francisco Pena-Pereira , Marek Tobiszewski , Wojciech Wojnowski , Elefteria Psillakis
{"title":"Corrigendum to: A Tutorial on AGREEprep an Analytical Greenness Metric for Sample Preparation","authors":"Francisco Pena-Pereira , Marek Tobiszewski , Wojciech Wojnowski , Elefteria Psillakis","doi":"10.1016/j.sampre.2022.100045","DOIUrl":"https://doi.org/10.1016/j.sampre.2022.100045","url":null,"abstract":"","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"4 ","pages":"Article 100045"},"PeriodicalIF":0.0,"publicationDate":"2022-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582022000420/pdfft?md5=c6c61151864fc9727af338670b2f1b91&pid=1-s2.0-S2772582022000420-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"92147506","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}