In this paper, we describe ultrasonic assisted-dispersive solid phase extraction based on ion-imprinted polymer (UA-DSPE-IIP) nanoparticles for the selective extraction of lead ions. Ultrasound is a good and robust method to facilitate the extraction of the target ions in the sorption step and elution of the target ions in the desorption step. The ion-imprinted polymer nanoparticles used in the UA-DSPE-IIP were prepared by precipitation polymerization technique. The ion-imprinted polymer nanoparticles was synthesized using 2-vinylpyridine as a functional monomer, ethylene glycol dimethacrylate as the cross-linker, 2,2′- azobisisobutyronitrile as the initiator, 1,3,4-thiadiazole-2,5-dithiol as the ligand, methanol/dimethyl sulfoxide as the solvent, and lead as the template ion, through precipitation polymerization technique. The IIP nanoparticles were characterized by Fourier transformed infra-red spectroscopy (FTIR), thermogravimetric and differential thermal analysis (TGA/DTA), and scanning electron microscopy (SEM). Box-Behnken design (BBD) was used for optimization of sorption and desorption steps in UA-DSPE-IIP. In the sorption step: pH of solution, IIP amount (mg), sonication time (min) for sorption and in the desorption step: concentration of eluent (mol L⁻¹), volume of eluent (mL), and sonication time (s) for desorption was investigated and optimized by the Box-Behnken design. The optimum conditions for the method were pH of solution: 7.5, sonication time for sorption 7.5 min, IIP amount 24 mg, type and concentration of eluent HCl 1.4 mol L⁻¹, volume of eluent 2.1 mL, and sonication time for desorption 135 s. Under the optimized conditions, the limit of detection and relative standard deviation for the detection of lead ions by UA-DSPE-IIP was found to be 0.7 μg L⁻¹ and <4%, respectively.

A novel ultrasound-assisted liquid phase microextraction (UALPME) based on environmental friendly extractants, deep eutectic solvent (DES) was first time presented for speciation of selenium. In present study, five DES solvents of different composition was prepared and used as efficient extractive medium for hydrophobic chelate of Se(IV) with 3,3′-Diaminobenzidine (DAB). The total inorganic Se species were determined after pre-reduction of Se(VI) to Se(IV), prior to applying developed method. The concentration of Se(VI) was calculated by the difference of Se(IV) values and total selenium contents. The concentration of Se in DES rich phase was measured with electrothermal atomic absorption spectrometer (ETAAS). The effects of different parameters on extraction efficiency of study analyte, including pH, ligand concentration, type and volume of DES, sonication time, volumes tetrahydrofuran and aqueous samples were examined. At the optimum conditions, limit of detection and quantification, preconcentration factor, and relative standard deviation (RSD %) were determined as 4.61ngL⁻¹, 15.4ngL⁻¹, 50% and 4.1%, respectively. The accuracy of the presented method was confirmed by analysis of certified reference material and standard addition method for different water and ice tea samples. The developed method was effectively applied to real water and food samples.

A novel green solvent-based ultrasonic assisted dispersive liquid–liquid microextraction (GS-UADLLME) method was developed for the preconcentration of cadmium and lead ions in various real samples prior to determination by graphite furnace atomic absorption spectrometry (GFAAS). In order to extract trace amounts of cadmium and lead ions, 2-amino-3-sulfhydrylpropanoic acid (l-cysteine) (as a green ligand), tetrafluoroborate ion (BF₄⁻) (as an ion pair agent) and 1-butyl-3-methylimidazolium tetrafluoroborate [BMIM][BF₄] (as acceptor phase) were used. Different effective factors in the microextraction procedure such as pH of the sample solution, sample solution volume, acceptor phase volume, l-cysteine and tetrafluoroborate concentrations, centrifugation conditions and salting addition were thoroughly optimized. Under the optimum conditions, the calibration graphs were linear in the range of 0.8–180 and 2.5–190 ng L⁻¹ with a correlation coefficient (r²) higher than 0.9967 for the measurement of cadmium and lead ions, respectively. The limits of detection for the determination of Cd(ii) and Pb(ii) for the proposed method were 0.2 and 0.7 ng L⁻¹, respectively. The relative standard deviations (n = 5) for the analyte determination were lower than 3.4%. In order to investigate the method’s accuracy, cadmium and lead contents of a certified reference material, SRM 1643e (NIST), were determined and the results from the proposed method were in very good agreement with the certified values. The suggested method was successfully applied to the determination of cadmium and lead ions in real samples such as real water, soil, rice and tea samples.