Combination of a dispersive solid phase extraction method based on octadecylamine modified magnetic nanoparticles with dispersive liquid–liquid microextraction for the extraction and preconcentration of pesticides

Abstract

In the present work, a new and efficient sorbent has been prepared using the co-precipitation method for magnetic dispersive solid phase extraction followed by dispersive liquid–liquid microextraction. This method was used for the extraction and preconcentration of some widely-used pesticides (chlorpyrifos, haloxyfop-R-methyl, oxadiazon, diniconazole, clodinafop-propargyl, fenpropathrin, and fenoxaprop-P-ethyl) from fruit juices prior to their determination by gas chromatography-flame ionization detection. The sorbent was prepared by octadecylamine co-precipitation with Fe₃O₄. In the first step, mg amount of the magnetic sorbent was spread into an aqueous sample solution including the selected analytes and vortexed. Then the analytes were eluted with acetonitrile from the surface of the nanoparticles separated with an external magnetic field from the aqueous solution. In the second step, the obtained eluent was mixed with an extraction solvent (chloroform) at the μL-level and rapidly injected into deionized water. After centrifugation, an aliquot of the sedimented phase was injected into the separation system. Experimental parameters which control the performance of both steps were investigated and optimized. Using optimum extraction conditions, the proposed method provided low limits of detection (0.23–0.41 μg L⁻¹) and quantification (0.81–1.3 μg L⁻¹), high enrichment factors (353–443), acceptable extraction recoveries (70–88%), and satisfactory relative standard deviations (≤6%) for intra- (n = 6) and inter-day (n = 4) precisions at a concentration of 30 μg L⁻¹ of each pesticide.