Magnetic solid-phase extraction of Zineb by C18-functionalised paramagnetic nanoparticles and determination by first-derivative spectrophotometry

Fe3O4-SiO2-C-18 paramagnetic nanoparticles have been synthesised and used as magnetic solid-phase extraction (MSPE) sorbent for the extraction of Zineb from agricultural aqueous samples under ultrasonic condition and quantified through a first-derivative spectrophotometric method. The produced magnetic nanoparticles were characterised by using scanning electron microscopy, X-ray diffraction spectroscopy, Fourier transform infrared spectroscopy and zeta potential reader. The Fe3O4-SiO2-C-18 paramagnetic nanoparticles had spherical structures with diameters in the range of 198-201nm. Further, MSPE was performed by dispersion of Fe3O4-SiO2-C-18 paramagnetic nanoparticles in a buffered aqueous solution accompanied by sonication. Next, the sorbents were accumulated by applying an external magnetic field and were washed with 4-(2-pyridylazo) resorcinol-dimethyl sulfoxide solution, for the purpose of desorbing the analyte. The extraction conditions (sample pH, washing and elution solutions, amount of sorbents, time of extraction, sample volume and effect of diverse ions), as well as Zineb-PAR first-order derivative spectra, were also evaluated. The calibration curve of the method was linear in the concentration range of 0.055-24.3mgL(-1) with a correlation coefficient of 0.991. The limit of detection and limit of quantification values were 0.022 and 0.055mgL(-1), respectively. The precision of the method for 0.27mgL(-1) solution of the analyte was found to be less than 3.2%. The recoveries of three different concentrations (0.27, 1.37 and 13.7mgL(-1)) obtained 98.3%, 98.5% and 96.0%, respectively. The proposed Fe3O4-SiO2-C-18 paramagnetic nanoparticles were found to have the capability of reusing for 7.0 times.