{"title":"Synthesis and application of iron based metal organic framework for efficient adsorption of azo dyes from textile industry samples","authors":"Kasturi Goswami, Megala Ulaganambi, Lokesh Kumar Sukumaran, Kishore K.R. Tetala","doi":"10.1016/j.sampre.2023.100080","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100080","url":null,"abstract":"<div><p>In this work, we have synthesized an iron based metal organic framework for removal of azo-dyes from textile industry wastewaters. The metal organic framework is comprised of two ligands, terephthalic acid and iminodiacetic acid chelated with iron. The chemical composition, surface morphology and diffraction pattern of the synthesized binary metal organic framework was confirmed with FT-IR, FE-SEM and XRD. Interaction with the model azo dye (methyl orange) has resulted in re-structuring of the native metal organic framework original shape (hexagonal nanorods to smaller octahedron structures). Under optimized conditions (time, and pH), the metal organic framework has a maximum methyl orange adsorption capacity of ∼ 280 mg per g. In presence of major salts as co-existing ions and two non-azo dyes, the methyl orange removal ability of metal organic framework significantly remained intact. The metal organic framework has displayed its practical applicability by efficiently removing two azo dyes (yellow and pink) from local textile industry wastewaters.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100080"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49765450","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}
María Vergara-Barberán , Laura Pont , Hiba Salim , Estela Giménez , Fernando Benavente
{"title":"On-line aptamer affinity solid-phase extraction capillary electrophoresis-mass spectrometry for the analysis of protein biomarkers in biological fluids and food: A tutorial","authors":"María Vergara-Barberán , Laura Pont , Hiba Salim , Estela Giménez , Fernando Benavente","doi":"10.1016/j.sampre.2023.100082","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100082","url":null,"abstract":"<div><p>The analysis by capillary electrophoresis (CE) of low abundant proteins in complex samples, such as biological fluids and food, is especially challenging, due to the poor concentration sensitivity of microscale separation techniques and the sample matrix complexity. In order to overcome these major drawbacks, microextraction sample preparation techniques based on on-line solid-phase extraction capillary electrophoresis (SPE-CE) are regarded as an excellent alternative for sample matrix clean-up and analyte preconcentration with minimum sample handling. In this study, we present, as a tutorial, a valve-free on-line aptamer affinity solid-phase extraction capillary electrophoresis-mass spectrometry (AA-SPE-CE-MS) method for purification, preconcentration, separation, detection, and characterization of intact protein biomarkers in biological fluids and food using as cases of study α‑synuclein (α‑syn), concanavalin A (Con A), and β-lactoglobulin (β-LG), which are related to Parkinson's disease and food allergy, respectively. This tutorial is not limited to the description of the analytical method, but it also provides ready-to-use preparation procedures for sorbent and microextraction devices, and introduces strategies to overcome undesired effects, allowing a straightforward implementation and optimum performance of AA-SPE-CE-MS, as a platform to develop further applications.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100082"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49758872","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}
Natalia Piqueras-García , María Vergara-Barberán , María Jesús Lerma-García , José Manuel Herrero-Martínez
{"title":"Aptamer-functionalized magnetic supports for sample preparation","authors":"Natalia Piqueras-García , María Vergara-Barberán , María Jesús Lerma-García , José Manuel Herrero-Martínez","doi":"10.1016/j.sampre.2023.100083","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100083","url":null,"abstract":"<div><p>In the last few years, aptamer-functionalized materials have been used as promising affinity sorbents for sample preparation purposes. These selective materials have attracted much attention due to their excellent molecular recognition properties, high stability, and the possibility of incorporation onto the surface of different supporting materials, such as nanoparticles, polymers, etc. On the other hand, current trends in extraction techniques encompass the use of miniaturized devices integrated with advanced affinity-based sorbents. Within these sample preparation devices, magnetic nanoparticles have become excellent candidates for the preparation of new functional nanomaterials for the solid-phase extraction processes. In addition to this approach, magnetic elements can be integrated in extraction devices (e.g., stir bars, stir cakes, etc.) to provide efficient extraction/stirring integrated techniques able to simplify the extraction and improve the performance. This review gives an overview of the literature published regarding aptamer-based sorbents using as host supports magnetic nanoparticles and integrated stirred units. For this purpose, the most relevant developments and applications achieved in the last seven years (from 2017 to 2023) in sample preparation by the integration of these affinity-based materials in extraction techniques such as magnetic solid-phase extraction and stir bar sorptive extraction will be reviewed.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100083"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49758873","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":"Advances in solvent-free sample preparation methods for matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) of polymers and biomolecules","authors":"Kayla Williams-Pavlantos, Chrys Wesdemiotis","doi":"10.1016/j.sampre.2023.100088","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100088","url":null,"abstract":"<div><p>Matrix assisted laser desorption ionization mass spectrometry (MALDI-MS) is an essential analytical technique for the molecular characterization of biomolecules and synthetic polymers. Its ability to provide comprehensive compositional information not afforded by other techniques, with high sensitivity and selectivity, is highly influenced by the sample preparation of the material prior to analysis. This review discusses MALDI-MS sample preparation protocols that do not utilize solvents. Such methods provide alternative routes for analyzing insoluble polymeric materials and may also reveal information that is not attainable with solvent-based sample preparation techniques. Additionally, this review will present relevant surface analysis and imaging results only achievable with solvent-free sample preparation methodologies.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100088"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49767318","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}
Fernando H. do Nascimento , Renan Vitek , Jorge C. Masini
{"title":"Porous polymer monoliths with complementary retention mechanisms for online solid-phase extraction liquid chromatography to determine lysozyme in egg white","authors":"Fernando H. do Nascimento , Renan Vitek , Jorge C. Masini","doi":"10.1016/j.sampre.2023.100069","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100069","url":null,"abstract":"<div><p>This work demonstrates the determination of lysozyme in egg-white samples after enrichment and cleanup by weak cation exchange (WCX) following separation by reversed-phase liquid chromatography (RPLC). The WCX column was prepared from glycidyl methacrylate (GMA) and ethylene glycol dimethacrylate (EDMA) and functionalized with iminodiacetate (IDA). Reversed-phase columns were prepared using butyl methacrylate (BMA) and EDMA. Photopolymerization formed the poly(GMA-co-EDMA) column inside vinylized polypropylene tubes whereas poly(BMA-co-EDMA) used thermal polymerization inside functionalized Silcosteel® tubes. The preparation of poly(GMA-co-EDMA) was fast (about 2 h), from preparing the polypropylene tube to washing the formed monolith with acetonitrile (ACN), but functionalization demanded an overnight period of pumping IDA through the column immersed in a water bath thermostated at 80 °C. Preparation of the poly(BMA-co-EDMA) also demanded overnight heating at 60 °C, with subsequent washing of the formed monolith with ACN. Egg-white samples diluted at a 1:10 m v<sup>−1</sup> ratio in phosphate buffer (pH 7.0) were injected first through IDA@poly(GMA-co-EDMA) to retain lysozyme (pI 11.4) and remove the proteins with a pI < 7.0. Elution of the lysozyme from the cation exchange column was made with 5% (v v<sup>−1</sup>) acetonitrile in 0.1% (v v<sup>−1</sup>) TFA. RPLC then analyzed the eluate with a gradient from 5 to 50% ACN in 0.1% TFA. The limits of detection and quantification were 0.07 and 0.23 mg mL<sup>−1</sup>, respectively. Egg-white lysozyme concentrations varied between 2.26 ± 0.06 and 4.41 ± 0.08 mg g<sup>−1</sup>, and spiking/recovery experiments at two concentration levels (0.25 and 0.50 mg mL<sup>−1</sup>) resulted in recoveries from 94 to 115%, thus demonstrating the columns working with orthogonal selectivity provided enrichment of less abundant lysozyme and accurate results, provided by an efficient cleanup of the sample matrix.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100069"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49759119","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":"Development of thin film microextraction method for the multi-residue analysis of selected pesticides","authors":"Kübra Kahremanoğlu , Yeliz Akpınar , Ezel Boyaci","doi":"10.1016/j.sampre.2023.100061","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100061","url":null,"abstract":"<div><p>Pesticides are a class of compounds that are used to protect agricultural products. However, the uncontrolled use of these chemicals increases the risks associated with their overdosing and rises a significant concern about their effect on human health and the ecosystem. Albeit many concerns about their effects, the use of pesticides is inevitable due to the incline in population growth and the presence of limited food resources. As a result, regulatory control of the use of chemicals is critical and the development of methods that provide a reliable determination of pesticide residues in fruits and vegetables is of great importance.</p><p>In the present study, a new method based on thin film microextraction was developed for the extraction of pesticides from fruit matrices prior to their gas chromatography-mass spectrometric (GC–MS) determination. As a first step, the thin film extractive devices were prepared by immobilization of hydrophilic-lipophilic balanced (HLB) particles on the surface of carbon mesh. The samplers were optimized in terms of extraction and desorption conditions first in PBS and then in apple juice. The final method was also validated in apple juice samples. Analytical figures of merits of the final method showed acceptable precision for intra- and inter-day reproducibility with ≤20% relative standard deviation (RSD%) and accuracy of ≤15% relative error (RE%), except for trifluralin at 300.0 ng mL<sup>−1</sup> level. The limits of quantitation (LOQ) for the selected pesticides were found between 1.0 and 5.0 ng mL<sup>−1</sup> . The samplers developed in this study were also successfully tested in preliminary investigations for the extraction of the pesticides from the surface of fruits and vegetables using agarose gel as a model matrix with the primary aim of showing the step towards the sampling directly on the field.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"6 ","pages":"Article 100061"},"PeriodicalIF":0.0,"publicationDate":"2023-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49727487","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-gas chromatography-mass spectrometry for the determination of favipiravir in biological and forensic samples","authors":"Rajeev Jain , Bharti Jain , Abuzar Kabir , Atul Bajaj , Ratnasekhar Ch , Shweta Sharma","doi":"10.1016/j.sampre.2023.100058","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100058","url":null,"abstract":"<div><p>Favipiravir, a pyrazine analog, is proposed as providential antiviral agent against the COVID-19 infection during 2020 pandemic emergency. For the first time, a fabric phase sorptive extraction (FPSE) combined with gas chromatography-mass spectrometry (GC-MS) has been developed and applied for the determination of favipiravir (FAV) in biological samples (human plasma, blood and urine), pharmaceutical and forensic samples. The method comprises of extraction of FAV by FPSE followed by its derivatization with N, O-bis (trimethylsilyl) trifluoroacetamide (BSTFA) and GC-MS analysis. Design of experiment-based optimization was performed using Placket-Burman Design (PBD) and Central Composite Design (CCD) for the screening of significant factors of FPSE and their optimization, respectively. Among all tested membranes, sol-gel polyethylene glycol (PEG) has offered the best extraction efficiency for FAV. Under optimum conditions, the proposed method was found to be linear in the range of 0.01–10 µg mL<sup>−1</sup> by GC-MS. The LODs and LOQs were as low as 0.001-0.0026 µg mL<sup>−1</sup> and 0.003-0.0086 µg mL<sup>−1</sup>, respectively by GC-MS. Intra-day and inter-day precisions were less than 5 and 10%, respectively, showing good method precision. The proposed method has been successfully applied to detect and quantify FAV in human urine, whole blood and plasma samples along with seized forensic samples. In addition, the proposed method has been evaluated for its green character by ComplexGAPI index.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"6 ","pages":"Article 100058"},"PeriodicalIF":0.0,"publicationDate":"2023-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49752962","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}
Guillem Peris-Pastor, Sandra Alonso-Rodríguez, Juan L. Benedé, Alberto Chisvert
{"title":"High-throughput determination of oxidative stress biomarkers in saliva by solvent-assisted dispersive solid-phase extraction for clinical analysis","authors":"Guillem Peris-Pastor, Sandra Alonso-Rodríguez, Juan L. Benedé, Alberto Chisvert","doi":"10.1016/j.sampre.2023.100067","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100067","url":null,"abstract":"<div><p>A reliable analytical method for the simultaneous determination of two oxidative stress biomarkers (i.e., 8‑hydroxy-2′-deoxyguanosine (8-oxodG) and 8‑hydroxy-2′-deoxyadenosine (8-oxodA)) in saliva samples is presented. These biomarkers are produced by an oxidative DNA damage and have gained prominence in the field of medicine as early diagnostic and disease control tools. The method is based on solvent-assisted dispersive solid-phase extraction (SA-DSPE) as a clean-up step, followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). For this purpose, a commercial polymer with a hydrophilic-hydrophobic balance has been used as extraction phase. This balance makes the material suitable for extracting compounds from polar matrices such as saliva. Those variables involved in the extraction were optimized by a Box-Behnken design, whereas those variables affecting the desorption were optimized by a Doehlert design, except the desorption solvent that was optimized by using a Simplex-Centroid design. The method was successfully validated, showing a good linearity at least up to 20 ng mL<sup>−1</sup>, limits of detection and quantification at the low ng mL<sup>−1</sup> level, and good precision values (< 15%). Standard addition calibration was employed to correct the observed matrix effects. Finally, this new approach was successfully applied to saliva samples from nine volunteers, three of them with type II diabetes, obtaining notable differences in the concentration values between both groups. The proposed methodology overcomes some of the drawbacks of the only previous work with the same purpose, such as the time-consuming procedure and the consumption of large volumes of organic solvents. To increase the sample throughput and reduce the analysis time, a thermostatic stirrer that allows the extraction of several samples simultaneously was used.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"6 ","pages":"Article 100067"},"PeriodicalIF":0.0,"publicationDate":"2023-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49752380","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}
Xue Ma , Lingyun Wang , Qingyun He , Qiannan Sun , Dan Yin , Yanhao Zhang
{"title":"A review on recent developments and applications of green sorbents-based solid phase extraction techniques","authors":"Xue Ma , Lingyun Wang , Qingyun He , Qiannan Sun , Dan Yin , Yanhao Zhang","doi":"10.1016/j.sampre.2023.100065","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100065","url":null,"abstract":"<div><p>Sample pretreatment is an essential step in the analytical process. Solid phase extraction (SPE) procedures are widely used for clean-up and enriching analytes in sample preparation due to the complex sample matrix and low concentration level of target compounds. The sorbent is the critical part and plays a vital role in the SPE process. The combination strategies of green sample preparation (GSP) with sorbents have been taken seriously to establish high-performance and environmental-friendly SPE methods. This work mainly reviewed the capacity of different functional materials to be used as SPE sorbents which fulfilled the GSP requirements, including metal-organic frameworks (MOFs), molecularly imprinted polymers (MIPs), natural products, and carbon-based materials. Advanced computer-assisted strategies for the synthesis and usage of green SPE sorbents are also overviewed. Finally, recent advanced applications of these green adsorption materials for SPE procedure were summarized. This review aims to retrace latest research of green sorbents-based SPE techniques under the perspective of GSP, suggesting the future synthesis and application of adsorption materials should pose the features of less reagent and energy usage, less labor and time consuming, and high extraction efficiency.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"6 ","pages":"Article 100065"},"PeriodicalIF":0.0,"publicationDate":"2023-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49752907","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}
Gema Casado-Hidalgo, Sonia Morante-Zarcero, Damián Pérez-Quintanilla, Isabel Sierra
{"title":"Magnetic material based on mesostructured silica functionalized with β-cyclodextrin to extract opium alkaloids in poppy seed infusions","authors":"Gema Casado-Hidalgo, Sonia Morante-Zarcero, Damián Pérez-Quintanilla, Isabel Sierra","doi":"10.1016/j.sampre.2023.100056","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100056","url":null,"abstract":"<div><p>Sample preparation methods tend to be fast, simple, with the use of new adsorbents and with lower amounts of organic solvents to make them more environmentally friendly. In this work, a magnetic solid-phase extraction (MSPE) protocol for the quantification of six opium alkaloids (OAs) in poppy seeds infusions has been optimised followed by analysis with liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). For this purpose, a mesostructured silica magnetic composite with β-CD (Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>@mSiO<sub>2</sub>@β-CD) was synthesised and characterized. To obtain the highest level of functionalisation, three proportions of β-CD monomer/material (12.5, 25 and 100%) were determined, demonstrating that 25% showed the highest level. Adsorption studies were carried out in water at different pH (1, 2, 7, 9 and 11) and times (1, 5, 10 and 20 min), confirming the high adsorption capacity at pH 9 for 1 min. Then, the elution conditions of MSPE procedure were optimised (50 mg material, 2 mL of water/EtOH at 50% with 1% formic acid for 1 min). The methodology was successful validated with low detection and quantification limits, negligible matrix effect and good recovery values (89–94%). The methodology was applied to analysis of home-made infusions with four different poppy seeds, observing in one of them a worrying amount of OAs which imply a content in the seeds of at least four times that of the legislation.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"6 ","pages":"Article 100056"},"PeriodicalIF":0.0,"publicationDate":"2023-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49752958","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}