Synthesis of ionically imprinted Poly(Alylthiourea) in the presence of 1-(2-Pyridylazo)-2-Napthol (PAN) for preconcentration in magnetic dispersive solid phase of nickel ions in water and food samples.

In the present study, a magnetic ion-imprinted polymer based on n-allylthiourea in the presence of 1-(2-pyridylazo)-2-naphthol (MIIP-PAN) was synthesized, characterized, and applied in the preconcentration of nickel ions by dispersive magnetic solid phase extraction (DMSPE) with FAAS detection. For comparison, non-imprinted polymer (MNIP-PAN) and imprinted polymer without PAN were synthesized. The characterization of the polymers was performed by FT-IR, DRX, TEM, TGA, VSM, and BET. Selectivity studies were performed comparing the competitive adsorption of Ni2+ with other cations on MIIP-PAN and MNIP-PAN, achieving higher relative selectivity coefficients for MIIP-PAN than for MNIP-PAN and NIP. Under optimized conditions, the method provided a preconcentration factor of 76.70, detection limit of 0.25 µg/L and intra-day (2.06 - 2.33 %) and inter-day (1.82 - 4.90 %) precision. The developed method was applied to samples of water, teas, and chocolate powder, and its precision was evaluated through tests of recovery and analysis of certified materials.

Vortex-assisted magnetic solid-phase extraction of cadmium in food, medicinal herb, and water samples using silica-coated thiol-functionalized magnetic multiwalled carbon nanotubes as adsorbent.

The current work focuses on the facile and effective synthesis of a new nanocomposite based on multiwalled carbon nanotubes (MWCNT) decorated with magnetic core-shell Fe3O4@SiO2 and functionalized with 3-mercaptopropyltrimethoxysilane (3-MPTS) used in the vortex-assisted dispersive magnetic solid-phase extraction (VA-DMSPE) of Cd(II) ions in environmental and food samples. The nanocomposite was characterized and the parameters that influenced the VA-DMSPE were optimized through a fractional factorial design 25-1. The proposed method provided a preconcentration factor of 33.14 times, detection and quantification limits of 0.090 µg L-1 and 0.302 µg L-1, respectively, and a linearity range of 0.001-40.0 µg L-1. The developed method was effectively applied to preconcentrate and determine Cd(II) in water, tobacco, green tea leaves, ginkgo biloba, carrots, and rice samples, and its accuracy was evaluated using GF AAS.