Magnetic solid-phase extraction coupled to high-performance liquid chromatography (HPLC)-diode array detection method has been developed for the sensitive analysis of Anastrozole (ANA) and Letrozole (LET) in human urine samples. Characterization studies of the newly synthesized material (Fe3O4@TEPA) were carried out by Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction, Raman spectroscopy, and scanning electron microscope techniques. The method has provided linearity for both the analytes (r2 > 0.9900) in the range of 4.00–160.00 ng mL−1. The limit of detections for ANA and LET was found to be 1.14 and 1.26 ng mL−1, respectively. The limit of quantification for ANA and LET was obtained 3.78 and 3.86 ng mL−1, respectively. The new method was simple, convenient, fast, and suitable for the direct analysis of ANA and LET in urine samples. Finally, the developed method was applied to the spiked human urine samples to test accuracy and repeatability. Recovery values for each of the molecules were calculated in the range of 93.4–108.0% (n = 3) at two concentration levels, while % RSDs were lower than 6.2%. Graphical abstract

Abstract

A new Polyacrylamide (PAA)-Vermiculite (V) composite was synthesized and characterized with the help of FTIR, SEM, and PZC analyses. The effects of ion concentration, pH and ionic strength parameters to adsorption process were investigated in detail. The obtained data were analyzed and discussed in the light of the Langmuir, Freundlich and Dubinin-Radushkevich (DR) models. It was shown that the adsorption of UO22+ increased with the increasing of the pH while the increasing or decreasing of the ionic strength did not lead to significant changes in adsorption process. The adsorption of uranyl ion on new designed material followed an endothermic and spontaneous process with increased disorderliness at adsorbate/adsorbent interface. It was noticed that the adsorption process exhibits a pseudo-second-order kinetics. The interaction mechanism regarding to the interaction between uranyl ion and new designed Polyacrylamide (PAA)-Vermiculite (V) composite was highlighted in the light of Density Functional Theory (DFT) calculations. Both theoretical and experimental analyses made proved that the designed new material with a adsorption capacity of 0.375 mol kg−1 is a potential adsorbent for effective removal of uranyl ions from solutions.