Preconcentration and spectrophotometric determination of low concentrations of malachite green and leuco-malachite green in water samples by high performance solid phase extraction using maghemite nanoparticles

A novel and sensitive extraction procedure using maghemite nanoparticles (γ-Fe₂O₃) modified with sodium dodecyl sulfate (SDS), as an efficient solid phase, was developed for removal, preconcentration and spectrophotometric determination of trace amounts of malachite green (MG) and leuco-malachite green (LMG). Combination of nanoparticle adsorption and easily magnetic separation was used to extraction and desorption of MG and LMG. The adsorption capacity was evaluated using both the Langmuir and Freundlich adsorption isotherm models. Maghemite nanoparticles were prepared by co-precipitation method and their surfaces were modified by SDS. The size and properties of the produced maghemite nanoparticles was determined by X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM) and BET analysis. MG and LMG became adsorbed at pH 3.0. LMG was oxidized to MG by adsorption on maghemite nanoparticles. The adsorbed MG was then desorbed and determined spectrophotometrically. The calibration graph was linear in the range 0.50-250.00 ng mL⁻¹ of MG and LMG with a correlation coefficient of 0.9991. The detection limit of the method for determination of MG was 0.28 ng mL⁻¹ and the relative standard deviation (R.S.D.) for 10.00 and 50.00 ng mL⁻¹ of malachite green was 1.60% (n = 3) and 0.86% (n = 5), respectively. A preconcentration factor of 50 was achieved in this method. The Langmuir adsorption capacity (q_max) was found to be 227.3 mg g⁻¹ of the adsorbent. The method was applied to the determination of MG in fish farming water samples.