Alberto Moral , Pol Clivillé-Cabré , Francesc Borrull , Kenneth G. Furton , Abuzar Kabir , Rosa Maria Marcé , Núria Fontanals
{"title":"Application of a homemade silica-based mixed-mode ion-exchange sorbent for the determination of drugs in environmental water samples","authors":"Alberto Moral , Pol Clivillé-Cabré , Francesc Borrull , Kenneth G. Furton , Abuzar Kabir , Rosa Maria Marcé , Núria Fontanals","doi":"10.1016/j.sampre.2023.100074","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100074","url":null,"abstract":"<div><p>Two homemade silica-based mixed-mode ion-exchange sorbents with strong moieties were compared for the solid-phase extraction (SPE) of a group of pharmaceuticals, drugs of abuse and metabolites. The difference between sorbents was the presence of graphene microparticles embedded in the network and the best results were obtained with the sorbent that did not contain graphene.</p><p>The optimum SPE protocol of the non-graphene sorbent was: loading pH at 3, different loading volumes depending on the type of sample, 2 mL of MeOH as washing solvent.</p><p>The optimized method was validated for the analysis of water samples of environmental interest (river water, effluent wastewater and influent wastewater). Apparent recoveries ranged from 22 to 68%, matrix effect values were lower than ±20 for most compounds, and method detection limits ranged from 1 to 28 ng/L and method quantification limits from 2 to 56 ng/L. Precision was obtained as percentual relative standard deviation (RSD%, n=4) and the repeatability and reproducibility between days were always lower than 18%.</p><p>The sorbent was used to determine the analytes in environmental water samples, where most compounds were found in the range from 2 to 180 ng/L in river samples, from 3 to 2547 ng/L in effluent wastewater samples and from 24 to 8086 ng/L in influent wastewater samples.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100074"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49750575","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}
Sergio J. Abellán-Martín , Jorge Pérez , Fernanda C. Pinheiro , Joaquim A. Nóbrega , Miguel Ángel Aguirre , Lorena Vidal , Antonio Canals
{"title":"Synergistic combination of natural deep eutectic solvent and chemical vapor generation for trace determination of As, Cd, Hg and Pb in drug samples by inductively coupled plasma optical emission spectrometry","authors":"Sergio J. Abellán-Martín , Jorge Pérez , Fernanda C. Pinheiro , Joaquim A. Nóbrega , Miguel Ángel Aguirre , Lorena Vidal , Antonio Canals","doi":"10.1016/j.sampre.2023.100084","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100084","url":null,"abstract":"<div><p>A new and environmentally friendly analytical method for simultaneous determination of As, Cd, Hg and Pb in drug samples by inductively coupled plasma optical emission spectrometry (ICP OES) has been developed. In order to increase the sensitivity of the analysis, a multinebulizer has been used for chemical vapor generation (CVG) after a dispersive liquid-liquid microextraction (DLLME) procedure using a natural deep eutectic solvent (NADES) as extractant solvent. The factors affecting analyte extraction and on-line chemical vapor generation have been optimized by multivariate analysis. Under optimized conditions, DLLME-CVG-ICP OES improved limit of quantitation (LOQ) values on average 50-fold higher compared with direct ICP OES analysis and afforded an increase of the sensitivity (i.e., enrichment factor) on average 25-times higher than those obtained with CVG-ICP OES analysis. According to the United States Pharmacopoeia (USP) Chapter 232, it means LOQ values are on average 4.3-times lower than their respective 0.3<em>J</em> values for the target-elements from class 1. Trueness has been evaluated by recovery experiments following USP recommendations for two oral drug samples in solid dosage form (i.e., commercial dosage tablets). In addition, the greenness of the developed method has been evaluated using the AGREEprep metrics, showing an excellent green character since it includes the miniaturization of the sample preparation procedure using a reduced volume (i.e., few microliters) of a non-hazardous extractant solvent for multielemental analysis.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100084"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49750702","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}
J. Bintanel-Cenis, L. Herrero, B. Gómara, L. Ramos
{"title":"Green fat removal in the analysis of polychlorinated biphenyls in biotic samples","authors":"J. Bintanel-Cenis, L. Herrero, B. Gómara, L. Ramos","doi":"10.1016/j.sampre.2023.100081","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100081","url":null,"abstract":"<div><p>A green analytical method based on the use of a deep eutectic solvent (DES) has been proposed for fat removal in the analysis of polychlorinated biphenyl (PCBs) in biotic samples. Using priority PCB congeners as model compounds, a novel sample preparation approach fully avoiding the use of mineral acids has been developed. Once optimized, the procedure allowed fat removal to be accomplished by 30min treatment with [chlorine chloride]:[oxalic acid dihydrated] 1:1 molar ratio at 60°C, with 3s vortexing every 5min to facilitate the homogenization of the slurry. Then, the target PCBs were recovered from the slurry by 20min extraction with 4mL of <em>n</em>-hexane. This DES-based method was combined with gas chromatography-quadrupole mass spectrometry (GC-qMS) for final PCB determination. The complete analytical method provided satisfactory recoveries of the target compounds (above 87% for all analytes), using as a small amount of sample as 0.150g. The repeatability of the complete procedure, expressed as relative standard deviation, was less than 5%, and the intermediate precision better than 14%. Final validation of the proposed methodology included the satisfactory comparison of the concentrations calculated for the endogenous PCBs in selected fatty foodstuffs with lipid contents under 18% (w/w fresh weight, fw) with those found when the same samples were analyzed by a more conventional and accepted reference procedure. The limits of detection were in all cases lower than 30 pg/g fw (as calculated for real samples), demonstrating the feasibility of the proposed procedure for accurate determination of the target compounds in biotic samples.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100081"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49758870","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}
Angel Puerta, Paula Tejedor-Matellanes, Inmaculada Luque-Jurado, Cristian Gonzalez-Jimenez, Ana Cristina Soria, Mercedes de Frutos
{"title":"Capillary electrophoresis instrumentation for determination of viscosity of deep eutectic solvents","authors":"Angel Puerta, Paula Tejedor-Matellanes, Inmaculada Luque-Jurado, Cristian Gonzalez-Jimenez, Ana Cristina Soria, Mercedes de Frutos","doi":"10.1016/j.sampre.2023.100086","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100086","url":null,"abstract":"<div><p>Deep eutectic solvents (DES), and especially natural deep eutectic solvents (NADES), are advantageous alternatives over non-environmentally friendly organic solvents traditionally employed for sample preparation in analytical chemistry. Moreover, the use of DES has recently experienced remarkable growth to fulfill the green analytical chemistry principles. One of their most influential characteristics, which should be determined for each new DES, is viscosity. Manual or automatic viscometers are usually employed to this aim, but their use is sometimes hampered by characteristics of DES such as their variable water content or their wide viscosity range. In this study a proof-of-concept of the feasibility of employing a capillary electrophoresis (CE) instrument to determine this physicochemical property is shown. No change in the commercial instrument is required, and advantages such as applying controlled pressure and temperature, online UV detection at several wavelengths, use of extremely low volumes of solvents and viscosity markers, automation, etc., allow the easy and affordable adaptation of this method to different DES. As example of application, CE methods were used for viscosity measurement of ten different DES, including hydrophilic (based on either choline chloride or betaine) and hydrophobic ones (based on thymol), within two orders of magnitude (6 to 500 mPa⋅s). Agreement between the experimental results obtained with the CE instrument and data gathered by a commercial viscometer adequate for solvents without water or with published data (when available), is shown. Contribution of using DES to the green analytical chemistry principles is reinforced by the characterization for the first time of these solvents with the more sustainable and high applicability CE method here proposed.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100086"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49767317","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}
Ainhoa Oller-Ruiz , Natalia Campillo , José Fenoll , Manuel Hernández-Córdoba , Pilar Viñas
{"title":"Dispersive magnetic solid-phase extraction for synthetic PDE-5 inhibitors determination by high-performance liquid chromatography with tandem mass spectrometry","authors":"Ainhoa Oller-Ruiz , Natalia Campillo , José Fenoll , Manuel Hernández-Córdoba , Pilar Viñas","doi":"10.1016/j.sampre.2023.100071","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100071","url":null,"abstract":"<div><p>A dispersive magnetic solid-phase extraction (DMPSE) procedure has been developed to preconcentrate four synthetic phosphodiesterase type 5 (PDE-5) inhibitors (sildenafil, desmethylsildenafil, vardenafil and tadalafil) from different samples (human hair, energy drinks, lubricating gels and dietary supplements). The target compounds were isolated from the solid samples by solid-liquid extraction in basic aqueous medium and the extract was submitted to DMSPE using multiwalled carbon nanotubes/Fe<sub>3</sub>O<sub>4</sub>@polypyrrole (MWCNTs/Fe<sub>3</sub>O<sub>4</sub>@PPy). For this, 20 mg of the magnetic nanocomposite was added to 30 mL of sample solution/extract and vortexed for 10 min before proceeding to the desorption step using 1 mL of methanol. Analysis was carried out by liquid chromatography with tandem mass spectrometry using electrospray ionization and a triple quadrupole mass analyzer (LC-ESI-QqQ-MS/MS). Matrix-matched calibration was applied for quantification. Limits of detection ranged between 0.01 and 0.22 ng mL<sup>−1</sup> for energy drinks and between 0.25 and 7.5 ng g<sup>−1</sup> for hair, lubricating gels, and dietary supplements. Relative standard deviations in the 4.3–12.2% (<em>n</em> = 10) were obtained for repeatability studies. The trueness of the proposed method was studied by fortifying the samples at two concentration levels and recoveries in the 85–112% range were obtained. None of the PDE-5 inhibitors studied were detected in real samples.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100071"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49750630","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}
Hao-Dong Wang , Nian Li , Jia-Hui Zhao , Bo Liu , Ning-Lan Xiao , Miao Zhang , Qiang Li , Hua-Jie Lai
{"title":"Synthesis of amphiphilic magnetic nanoparticles for highly efficient enrichment of steroid hormones in aquatic environment","authors":"Hao-Dong Wang , Nian Li , Jia-Hui Zhao , Bo Liu , Ning-Lan Xiao , Miao Zhang , Qiang Li , Hua-Jie Lai","doi":"10.1016/j.sampre.2023.100078","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100078","url":null,"abstract":"<div><p>The steroid hormones in the aquatic environment have attracted widespread attentions due to their harmful effects to organisms. In order to improve the sensitivity and accuracy of steroid hormone detection, amphiphilic magnetic nanoparticles (AMNPs) were prepared through suspension copolymerization for microSPE of steroid hormones in water. The divinylbenzene and N-vinylpyrrolidone were selected as modified monomers, and Fe<sub>3</sub>O<sub>4</sub> as the magnetic core. The FT-IR and SEM analyses showed that amphiphilic modified polymers were successfully coated on the surface of Fe<sub>3</sub>O<sub>4</sub> magnetic beads. The hysteresis loop showed that the saturation magnetization value of obtained AMNPs was 36 emu·<em>g</em><sup>−</sup><sup>1</sup>. In the adsorption test, the adsorption rate of nine steroid hormones by AMNPs can reach more than 90%. Based on this, an AMNPs-microSPE coupled with HPLC-MS/MS method was established to detect steroid hormones in the aquatic environment. The detection limit and quantitation limit of this analytical method was 0.01–0.72 μg·<em>L</em><sup>−</sup><sup>1</sup> and 0.10–2.4 μg·<em>L</em><sup>−</sup><sup>1</sup> respectively, with good linear fit and low relative standard deviation. The prepared AMNPs extraction materials show good recovery and reproducibility for steroid hormones in water, and have the advantages of low price, easy availability and reusable.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"7 ","pages":"Article 100078"},"PeriodicalIF":0.0,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49758867","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":"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}