Overview of the novel sorbents available in solid-phase extraction to improve the capacity and selectivity of analytical determinations

Aquest article descriu els nous desenvolupaments en materials polimèrics que milloren l'extracció en fase sòlida (SPE) dels anàlits presents en mostres líquides. Se centra principalment en nous sorbents polimèrics, tant els comercialment disponibles com els sintetitzats per grups de recerca, amb propietats millorades per a l'extracció d'analits. Es descriuen diversos tipus de sorbents polimèrics, des dels que milloren la capacitat d'extracció (anomenats hypercrosslinked, amb elevada àrea superficial i hidrofilicitat) fins als que milloren la selectivitat del procés (els polímers d'empremta molecular [MIP] sintetitzats amb una cavitat específica per a l'analit d'interès) i també aquells que combinen ambdues propietats (coneguts com sorbents de mode mixt, que són sorbents d'elevada capacitat amb un grup d'intercanvi iònic que aporta la selectivitat en el procés d'extracció). També es presenten i es comparen resultats dels diversos sorbents quan s'apliquen a SPE d'analits en matrius dels camps d'aplicació analítics més rellevants.This article provides an overview of the most recent developments in polymer materials that improve the solidphase extraction (SPE) of analytes from liquid samples. The main focus is on new polymeric sorbents, both commercially available and “in-house” synthesized, whose enhanced properties allow suitable extraction. Several types of polymeric sorbents are described herein. Hypercrosslinked sorbents improve the capacity of the extraction process due to their large specific surface areas and balanced hydrophilicities. Molecularly imprinted polymers (MIPs) are synthesized with a specific cavity for the analyte of interest, improving extraction selectivity. Another type are mixed-mode sorbents that are high-capacity sorbents that contain an ion-exchange moiety that finetunes the selectivity of the extraction process. Finally, the results obtained when these sorbents are applied as SPE material to extract analytes in different liquid matrices are presented and comparatively discussed in the context of the most relevant analytical fields

La enseñanza del inglés como lengua extranjera basada en contenidos

Aquest article recull les dades d’un estudi empíric sobre les percepcions del professorat de secundària de les Illes Balears en relació amb l’aprenentatge integrat de continguts i llengua estrangera. En concret, l’objectiu principal de l’estudi és el de detectar el grau de familiarització del professorat d’educació secundària amb la metodologia de l’ensenyament de llengües basada en continguts i la freqüència d’ús. Els resultats que aquí s’exposen provenen de l’anàlisi d’un qüestionari elaborat per l’equip d’investigació i distribuït al professorat d’anglès de batxillerat a les Illes Balears. Un total de 90 professors participaren en l’experiència, fet que constitueix una mostra representativa d’aquesta població educativa. Els resultats apunten a una familiarització del professorat amb els mètodes d’ensenyament de llengües basats en continguts, als quals s’atribueix gran efectivitat, si més no tenen una implantació encara escassa en el nostre entornEl presente artículo recoge los datos de un estudio empírico sobre las percepciones del profesorado de secundaria de las Islas Baleares en relación con el aprendizaje integrado de contenidos y lengua extranjera. En concreto, el objetivo principal del estudio es detectar el grado de familiarización del profesorado de educación secundaria con la metodología de la enseñanza de lenguas basada en contenidos y la frecuencia de uso de la misma. Los resultados que aquí se presentan provienen del análisis de un cuestionario elaborado por el equipo de investigación y distribuido al profesorado de inglés de bachillerato en las Islas Baleares. Un total de 90 profesores participaron en la experiencia, lo que constituye una muestra representativa de dicha población educativa. Los resultados apuntan a una familiarización del profesorado con los métodos de enseñanza de lenguas extranjeras basados en contenidos, a los que se atribuye gran efectividad, si bien tienen una implantación todavía escasa en nuestro entorn

Hypercrosslinked polymer microspheres decorated with anion- and cation-exchange groups for the simultaneous solid-phase extraction of acidic and basic analytes from environmental waters

Mixed-mode ion-exchange sorbents were introduced to improve the selectivity and retention of solid-phase extraction (SPE) sorbents,. Mixed-mode ion-exchange sorbents integrate reversed-phase chemistry with ion-exchange groups to promote favourable interactions with ionic species. Nevertheless, a need to extract analytes with acidic and basic properties simultaneously within the same SPE cartridge led to the introduction of novel amphoteric/zwitterionic sorbents, which incorporate cation- and anion-exchange moieties within the same functional group attached to the polymeric network. In the present study, the development, preparation and SPE evaluation of two novel hypercrosslinked zwitterionic polymeric sorbents, functionalised with either strong anion-exchange (SAX) and weak cation-exchange (WCX) or weak anion-exchange (WAX) and strong cation-exchange (SCX) groups (namely HXLPP-SAX/WCX and the HXLPP-WAX/SCX), is presented for the simultaneous retention of acidic and basic compounds. The sorbents were prepared by a precipitation polymerisation route which yielded poly(divinylbenzene-co-vinylbenzylchloride) as a precursor polymer; subsequently, the precursor polymer was hypercrosslinked, to increase the specific surface areas and capacities of the sorbents, and then functionalised to impart the zwitterionic character. The HXLPP-SAX/WCX sorbent was decorated with quaternised sarcosine groups and the HXLPP-WAX/SCX sorbent was decorated with taurine moieties. The SPE parameters were optimised to exploit the ionic interactions between compounds and the functional groups. The optimal conditions involve a washing step to remove the compounds retained by hydrophobic interactions, thus increasing the selectivity. The optimised SPE protocol used the quaternised sarcosine-based sorbent followed by liquid chromatography and tandem mass spectrometry, and was applied to determine compounds with acidic and basic properties from environmental samples, such as river water and effluent wastewater samples, with excellent selectivity and matrix effect values below -30% and apparent recovery results ranging from 52% to 105% for most of the compounds. The analytical method was validated for environmental water samples and used in the analysis of samples in which some of the target compounds were found at ng L−1 concentration levels

Microporous polymer microspheres with amphoteric character for the solid-phase extraction of acidic and basic analytes

Solid-phase extraction (SPE) is a widely-used and very well-established sample preparation technique for liquid samples. An area of on-going focus for innovation in this field concerns the development of new and improved SPE sorbents that can enhance the sensitivity and/or the selectivity of SPE processes. In this context, mixed-mode ion-exchange sorbents have been developed and commercialised, thereby allowing enhanced capacity and selectivity to be offered by one single material. The ion-selectivity of these materials is such that either anion-exchange or cation-exchange is possible, however one limitation to their use is that more than one sorbent type is required to capture both anions and cations. In this paper, we disclose the design, synthesis and exploitation of a novel SPE sorbent based on microporous polymer microspheres with amphoteric character. We show that it is possible to switch the ion-exchange retention mechanism of the sorbent simply by changing the pH of the loading solution; anion-exchange dominates at low pH, cation-exchange dominates at high pH, and both mechanisms can contribute to retention when the polymer-bound amphoteric species, which are based on the α–amino acid sarcosine (N-methylglycine), are in a zwitterionic state. This is an interesting and useful feature, since it allows distinctly different groups of analytes (acids and bases) to be fractionated using one single amphoteric sorbent with dual-functionality. The sarcosine-based sorbent was applied to the SPE of acidic, basic and amphoteric analytes from ultrapure water, river water and effluent wastewater samples. Under optimised conditions (loading 100 mL of sample at pH 6, washing with 1 mL of MeOH and eluting with an acidic or basic additive in MeOH) the recoveries for most of the compounds were from 57% to 87% for river water and from 61% to 88% for effluent wastewater. We anticipate that these results will lay the basis for the development of a new family of multifunctional sorbents, where two or more separation mechanisms can be embedded within one single, bespoke material optimised for application to challenging chemical separations to give significant selectivity advantages over essentially all other state-of-the-art SPE sorbents

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A new tool of Corporate Communication for the Documentation Degree is presented. It's Docublog, the first weblog of an Information Science Degree in Catalonia http://docublog.blogs.uoc.edu

Overview of the novel sorbents available in solid-phase extraction to improve the capacity and selectivity of analytical determinations

Aquest article descriu els nous desenvolupaments en materials polimèrics que milloren l’extracció en fase sòlida (SPE) dels anàlits presents en mostres líquides. Se centra principalment en nous sorbents polimèrics, tant els comercialment disponibles com els sintetitzats per grups de recerca, amb propietats millorades per a l’extracció d’analits. Es descriuen diversos tipus de sorbents polimèrics, des dels que milloren la capacitat d’extracció (anomenats hypercrosslinked, amb elevada àrea superficial i hidrofilicitat) fins als que milloren la selectivitat del procés (els polímers d’empremta molecular [MIP] sintetitzats amb una cavitat específica per a l’analit d’interès) i també aquells que combinen ambdues propietats (coneguts com sorbents de mode mixt, que són sorbents d’elevada capacitat amb un grup d’intercanvi iònic que aporta la selectivitat en el procés d’extracció). També es presenten i es comparen resultats dels diversos sorbents quan s’apliquen a SPE d’analits en matrius dels camps d’aplicació analítics més rellevants.This article provides an overview of the most recent developments in polymer materials that improve the solid-phase extraction (SPE) of analytes from liquid samples. The main focus is on new polymeric sorbents, both commercially available and “in-house” synthesized, whose enhanced properties allow suitable extraction. Several types of polymeric sorbents are described herein. Hypercrosslinked sorbents improve the capacity of the extraction process due to their large specific surface areas and balanced hydrophilicities. Molecularly imprinted polymers (MIPs) are synthesized with a specific cavity for the analyte of interest, improving extraction selectivity. Another type are mixed-mode sorbents that are high-capacity sorbents that contain an ion-exchange moiety that finetunes the selectivity of the extraction process. Finally, the results obtained when these sorbents are applied as SPE material to extract analytes in different liquid matrices are presented and comparatively discussed in the context of the most relevant analytical fields

Materials for Solid-Phase Extraction of Organic Compounds

This review provides an overview of the most recent developments involving materials for solid-phase extraction applied to determine organic contaminants. It mainly concerns polymer-based sorbents that include high-capacity, as well as selective sorbents, inorganic-based sorbents that include those prepared using sol-gel technology along with structured porous materials based on inorganic species, and carbon nanomaterials, such as graphene and carbon nanotubes. Different types of magnetic nanoparticles coated with these materials are also reviewed. Such materials, together with their main morphological and chemical features, are described, as are some representative examples of their application as solid-phase extraction materials to extract organic compounds from different types of samples, including environmental water, biological fluids, and food

Selective determination of pharmaceuticals and illicit drugs in wastewaters using a novel strong cation-exchange solid-phase extraction combined with liquid chromatography–tandem mass spectrometry

In this study, two materials are presented with strong cation-exchange (SCX) behaviour synthesised by two different approaches and then crushed for their application as sorbents for solid-phase extraction (SPE) to extract a group of pharmaceuticals and illicit drugs selectively from wastewater samples. The first SCX polymer was obtained by copolymerisation of three monomers: 2-acrylamido-2-methylpropane sulphonic acid (AMPSA), 2-hydroxyethyl methacrylate (HEMA) and pentaerythritol triacrylate (PETRA), while the second was obtained by post-modification with sulphuric acid (H2SO4) of a copolymer based on HEMA and divinylbenzene (DVB). After their syntheses, both polymers were evaluated as SPE sorbents, with all parameters affecting SPE being optimised, such as sample pH, washing and elution solvents and volumes. Thanks to the sulphonic groups present in the structure of the polymers, all of the compounds with basic functionalities were retained on the sorbents after the washing step, removing the acidic analytes and other interfering compounds, providing successful results in terms of ion suppression/enhancement (-12% and 21%) when wastewater samples were analysed. However, AMPSA/HEMA/PETRA (20/60/20) failed to retain the analytes after loading wastewater samples (25 or 50 mL), decreasing analyte recovery values significantly, whereas the sulphonated HEMA/DVB (50/50) enabled good SPE performance with recovery values between 70% and 98%, except for ranitidine and EDDP (39% and 43%, respectively). Therefore, this polymer was selected for further method validation and quantification of wastewater samples, providing low method detection limits (MDLs) in this matrix (from 2 to 40 ng L−1). Finally, most of the studied compounds were detected and quantified in wastewater samples, especially atenolol, ranitidine, cocaine and its metabolite benzoylecgonine

Ceramic passive samplers for determining pharmaceuticals and drugs of abuse in river and drinking water

An important challenge today is to efficiently monitor the presence of polar pharmaceuticals and drugs in surface and drinking waters to ensure its safeness. Most studies rely on grab sampling techniques, which enable the determination of contaminants at a given point and given time. In this study, we propose the use of ceramic passive samplers (CPSs) to increase the representativeness and efficiency of organic contaminant monitoring in waters. Firstly, we have assayed the stability of 32 pharmaceuticals and drugs and found that five of those compounds were unstable. Moreover, we evaluated the retention capabilities of three sorbents (Sepra ZT, Sepra SBD-L, and PoraPak Rxn RP) in solid-phase extraction (SPE) mode and found no differences in terms of recoveries for all three sorbents. We then calibrated CPSs using the three sorbents for the 27 stable compounds over 13 days, with a suitable uptake for 22 compounds with sampling rates between 0.4 and 17.6 mL/day, which indicates high uptake efficiency. CPSs with the Sepra ZT sorbent were deployed in river water (n = 5) and drinking water (n = 5) for 13 days. Some of the studied compounds occurred with a time-weighted concentration, for instance, of 43 ng/L for caffeine, 223 ng/L for tramadol or 175 ng/L for cotinine in river water.The authors would like to acknowledge financial support received from ACCIO of the Generalitat de Catalunya and the European Regional Development Fund (ERDF) under project COMRDI16-1-0063, and from MCIN/AEI/10.13039/501100011033 and the European Regional Development Fund (ERDF) under projects PID2020-114587GB-I00 and PID2019-105732GBC21 and the Severo Ochoa project Grant CEX2018-000794-S to IDAEA-CSIC as Centre of Excellence.Peer reviewe