Magnetic Polyamide Nanocomposites for the Microextraction of Benzophenones from Water Samples.

In this article, the influence of the monomers on the extraction efficiency and the effect of the addition of surfactants during the synthesis have also been considered. The sorption capacity of the resulting nanocomposites has been evaluated, in the dispersive micro-solid phase extraction format, by determining that of six benzophenones in water using ultra performance liquid chromatography (UPLC) combined with photodiode array detection. Under the optimum conditions, the limits of detection were in the range of 0.5⁻4.3 ng/mL and the repeatability, expressed as the relative standard deviation (RSD), varied between 1.5% and 5.6%. The proposed method has been applied for the analysis of real water samples, providing relative recoveries in the interval of 84⁻105.

Recycling polymer residues to synthesize magnetic nanocomposites for dispersive micro-solid phase extraction.

The ubiquitous presence of plastics, an obvious consequence of their usefulness and low price, has turned them into a problem of environmental and safety concern. The new plastic economy, an initiative recently launched by the World Economic Forum and Ellen MacArthur Foundation, with analytical support from McKinsey & Company, promotes a change in the use of plastic worldwide around three main pillars: redesign, reusing and recycling. Recycled plastics, with the aim of extending their life spam, can be used to synthesize materials for analytical purposes. In this article polystyrene (PS) trays, previously used for food packaging, are proposed as polymeric source for the synthesis of magnetic nanocomposites. The synthesis plays with the solubility of PS in different solvents in such a way that PS is gelated in the presence of cobalt ferrite nanoparticles which are finally embedded in the polymeric network. The extraction capability of the magnetic PS nanocomposite was evaluated using the determination of four parabens (methylparaben, ethylparaben, propylparaben and butylparaben) in water using liquid chromatography-tandem mass spectrometry as model analytical problem. Under the optimum conditions, limits of detection and quantification were in the range of 0.05-0.15 and 0.15-0.5ng/mL, respectively. The precisions, expressed as relative standard deviation (RSD), varied between 4.4% and 8.5% and the relative recoveries for analysis of the water samples were in the interval 81.2-104.5%.

Determination of propranolol and carvedilol in urine samples using a magnetic polyamide composite and LC-MS/MS.

AIM: ß-blockers are compounds that bind with adrenoreceptors hindering their interaction with adrenalin and noradrenalin. They are clinically relevant and they are also used in some sport as doping agents. RESULTS: A new method based on the combination of dispersive micro-solid phase extraction and LC-MS/MS has been developed to determine propranolol and carvedilol in urine samples. For this purpose a magnetic-polyamide composite is synthesized and used as sorbent. Working under the optimum conditions, the method provides limits of detection and quantification in the range of 0.1-0.15 µg/l and 0.3-0.5 µg/l, for carvedilol and propranolol, respectively. The precision, expressed as RSD, was better than 9.6% and the relative recoveries varied between 73.7 and 81.3%. CONCLUSION: The methodology is appropriate for the determination of ß-blockers in urine samples at the low microgram per liter range for therapeutic purposes.

Octadecyl functionalized core-shell magnetic silica nanoparticle as a powerful nanocomposite sorbent to extract urinary volatile organic metabolites.

In this present study, magnetic Fe3O4@SiO2 nanoparticles (MNPs) functionalized with octadecyl groups (Fe3O4@SiO2-C18 NPs) were synthesized, characterized and employed, for the first time, as powerful nanosorbent to extract endogenous volatile organic metabolites (EVOMs) namely, hexanal, heptanal, decanal, benzaldehyde, 4-heptanone, 5-methyl-2-furfural and phenol, described as potential biomarkers of cancer, from human urine. By using co-precipitation, surface modification methods, the carbon-ferromagnetic nanocomposite was synthesized and characterized by infrared spectrum (IR) and transmission electron microscopy (TEM). By coupling with gas chromatography-mass spectrometry (GC-qMS), a reliable, sensitive and cost-effective method was validated. To test the extraction efficiency of the carbon-ferromagnetic nanocomposite toward urinary EVOMs experimental variables affecting the extraction performance, including nanosorbent amount, adsorption time, elution time, and nature of elution solvent, were investigated in detail. The extraction process was performed by dispersing Fe3O4@SiO2-C18 NPs into working solution containing targeted VOMs, and into urine samples, and then eluted with an adequate organic solvent. The eluate was collected, concentrated and analyzed by GC-qMS. Under the optimized conditions, the LODs and LOQs achieved were in the range of 9.7-57.3 and 32.4-190.9ng/mL, respectively. Calibration curves were linear (r(2)≥0. 988) over the concentration ranges from 0.25 to 250ng/mL. In addition, a satisfying reproducibility was achieved by evaluating the intra- and inter-day precisions with relative standard deviations (RSDs) less than 3 and 11%, respectively. The method also afforded satisfactory results in terms of the matrix effect (72.8-96.1%) and recoveries (accuracy) higher than 75.1% for most of the studied EVOMs. The Fe3O4@SiO2-C18 NPs-based sorbent extraction combined with GC-qMS revealed that the new nanosorbent had a strong ability to retain the target metabolites providing a new, reliable and high throughput strategy for isolation of targeted EVOMs in human urine, suggesting their potential to be applied in other EVOMs.

Magnetic nanoparticles-nylon 6 composite for the dispersive micro solid phase extraction of selected polycyclic aromatic hydrocarbons from water samples.

In this article, the easy synthesis of magnetic nanoparticles-nylon 6 composite is presented, characterized and applied in the microextraction field. The one-step synthesis of the composite is performed by a solvent changeover playing with the different solubility of the polymeric network in formic acid and water. The new material has been characterized by different techniques including infrared spectroscopy, transmission and scanning microscopy. The extraction performance of the composite under a dispersive micro solid phase extraction format has been evaluated by determining four polycyclic aromatic hydrocarbons (benzo[b]fluoranthene, fluoranthene, indeno[1,2,3-cd]pyrene and phenanthrene) in water using ultra performance liquid chromatography (UPLC) combined with photo diode array detection. The developed methodology allows the determination of the analytes with limits of detection in the range from 0.05 µg/L (benzo[b]fluoranthene) to 0.58 µg/L (phenanthrene). The repeatability of the method was better than 6.9% at the limit of quantification level. The relative recoveries varied in the interval 80-111%.

Hybridization of commercial polymeric microparticles and magnetic nanoparticles for the dispersive micro-solid phase extraction of nitroaromatic hydrocarbons from water.

In this article, the combination of commercial polymeric microparticles (OASIS MCX) and cobalt ferrite nanoparticles is evaluated in dispersive micro-solid phase extraction (D-µSPE) for the determination of six nitroaromatic hydrocarbons in water. The high affinity of the polymeric material toward the target analytes as well as the magnetic behavior of cobalt ferrite nanoparticles are combined in a synergic way to developed an efficient and simple D-µSPE approach. The sorptive performance of the hybrid material is compared with that most usual sorbents and the effect of its synthesis steps on the extraction capability is also evaluated in depth. After the optimization of selected variables, D-µSPE method was assessed in terms of linearity, sensitivity, precision and accuracy. The new extraction method allows the determination of the target compounds with limits of detection in the range from 0.12 to 1.26 µg/L and relative standard deviations lower than 9.6%. The recovery study was performed in two different water samples obtaining percentages from 71 to 103%, which demonstrated the applicability of the hybrid sorbent for the selected analytical problem.