Magnetism-assisted in-tube solid phase microextraction based on porous monolith mingled with Fe 3 O 4 nanoparticles was developed for capture of phenolic acids in fruit juices. First, poly (1-allyl-3-methylimidazolium bis [(trifluoro methyl) sulfonyl] imide-co-ethylene dimethacrylate) monolith embedded with Fe 3 O 4 nanoparticles was facile fabrication in a capillary and employed as microextraction column. Subsequently, a magnetic coil adopted to produce variable magnetic fields during extraction stage was twined on the microextraction column. The analytes contents in eluant were quantified by high performance liquid chromatogram with diode array detector. Various parameters affecting the extraction performance were inspected and optimized in detail. Results revealed that the exertion of magnetic fields in adsorption and desorption steps enhanced the extraction efficiencies of analytes from 44.9-64.0% to 78.6-87.1%. Under the optimal extraction factors, the limits of detection were between 0.012 and 0.061 μg/L, relative standard deviations for precision in terms of intra-and inter-day assay variability ranged from 1.9 to 9.8%. The introduced approach was successfully applied to simultaneously quantify the contents of five analytes in real fruit juices with satisfying fortified recoveries (80.1-116%). The obtained results well demonstrate the promising potential of the developed method in the highly sensitive quantification of trace phenolic acids in complex samples.
In this study, a new adsorbent based on monolith/aminated carbon nanotubes composite was facilely prepared and employed as the extraction phase of multiple monolithic fibers solid-phase microextraction for the capture of phenoxycarboxylic acids herbicides. The adsorbent was fabricated by mingling aminated carbon nanotubes in the poly (allylthiourea-co-ethylene glycol dimethacrylate) monolith. Various techniques were employed to characterize the morphology, structure, and pore size of the prepared adsorbent. The proposed microextraction method displayed satisfactory capture performance towards studied analytes through multi-interactions such as hydrogen-bonding, hydrophobic and π-π interactions. Under the optimized conditions, a sensitive and reliable method to quantify trace analytes in water and soil samples was developed. The limits of detection were in the ranges of 0.13-0.25 μg/L and 0.20-0.61 μg/kg for water and soil samples, respectively. The practicality of the introduced method was demonstrated by applying it to monitor the contents of studied analytes in environmental water and soil samples. Satisfactory fortified recoveries (76.4-119%) and reproducibility were obtained. The achieved results well demonstrated that the suggested microextraction technique can efficiently extract phenoxycarboxylic acids and the developed method exhibits a promising potential for reliable and sensitive quantification of trace analytes in complex samples.
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