Abstract

In this study, the new synthesized magnetic nanoparticles based on amorphous carbon have been used as a sorbent in magnetic dispersive solid-phase extraction prior to dispersive liquid-liquid micro-extraction. The developed method was applied for analysis of ten pesticides from different fruit juice samples by gas chromatography-flame ionization detection. In this work, a few mg of the sorbent is added into an aqueous solution containing the analytes. Adsorption and desorption of the compounds of interest are accelerated by vortexing and sonication, respectively. To achieve high enrichment factors, a suitable organic solvent (iso-propanol) is used to elute the target analytes from the nanosorbent. The obtained iso-propanol is phased and 1,1,2-trichloroethane are employed as the disperser and extraction solvents, respectively, in the following micro-extraction procedure. The synthesized magnetic nanoparticles were characterized by scanning electron microscope, X-ray diffraction, vibrating sample magnetometer, and Fourier-transform infrared spectrophotometer. To achieve the high extraction efficiency and optimum conditions, all parameters that could affect the extraction yield were investigated. Under optimum conditions, the method had broad linear ranges with a proper linearity (r2 ≥ 0.9987). Limits of detection and quantification for analysis of the selected pesticides were found in the ranges of 0.5-1.0 and 1.7-3.3µg L-1, respectively. High enrichment factors and extraction recoveries were obtained in the ranges of 321-438 and 64-88%, respectively. To evaluate repeatability of the method, it was performed on two sets of standard solutions at the concentrations of 10 and 50µg L-1 (each analyte). Relative standard deviations varied in the ranges of 2-6% and 4-7% for intra- (n = 6) and inter-day (n = 5) precisions, respectively.

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