ABSTRACT
In the present study, ionic liquid-modified silica-coated magnetic nanoparticles (Fe3O4@SiO2@IL) were synthesized and applied as adsorbents for extraction and determination of paraquat (PQ) followed by high-performance liquid chromatography. For assurance of the extraction efficiency, the obtained results were compared with those obtained by bared magnetic nanoparticles (MNPs). Experimental design and response surface methodology were used for optimization of different parameters which affect extraction efficiency of paraquat using both adsorbents. Under the optimized conditions, extraction recoveries in the range of 20-25 and 35-40 % with satisfactory repeatability values (RSDs%, n = 4) less than 5.0 % were obtained for bared MNPs and Fe3O4@SiO2@IL, respectively. The limits of detection were 0.1 and 0.25 µg/L using Fe3O4@SiO2@IL and bared MNPs, respectively. The linearity was obtained in the range of 0.25 to 25 µg/L and 0.5 to 25 µg/L for Fe3O4@SiO2@IL and bared MNPs, respectively, with the coefficients of determination better than 0.9950. Finally, Fe3O4@SiO2@IL was chosen as superior adsorbent due to more dispersion ability, higher extraction recovery, lower detection limit, as well as better linearity and repeatability. Calculated errors (%) were in the range of 3 to 10 % depicting acceptable accuracy for the analysis of PQ by the proposed method. Finally, the method was successfully applied for extraction and determination of PQ in some water and countryside soil samples.
Subject(s)
Ionic Liquids/chemistry , Magnetite Nanoparticles/chemistry , Paraquat/isolation & purification , Silicon Dioxide/chemistry , Soil Pollutants/analysis , Solid Phase Extraction/methods , Water Pollutants, Chemical/analysis , Adsorption , Chromatography, High Pressure Liquid/methods , Limit of Detection , Magnetics , Microscopy, Electron, Scanning , Paraquat/analysis , Reproducibility of Results , Surface PropertiesABSTRACT
In this study, a simple and rapid extraction method based on the application of polypyrrole-coated Fe3 O4 nanoparticles as a magnetic solid-phase extraction sorbent was successfully developed for the extraction and preconcentration of trace amounts of formaldehyde after derivatization with 2,4-dinitrophenylhydrazine. The analyses were performed by high-performance liquid chromatography followed by UV detection. Several variables affecting the extraction efficiency of the formaldehyde, i.e., sample pH, amount of sorbent, salt concentration, extraction time and desorption conditions were investigated and optimized. The best working conditions were as follows: sample pH, 5; amount of sorbent, 40 mg; NaCl concentration, 20% w/v; sample volume, 20 mL; extraction time, 12 min; and 100 µL of methanol for desorption of the formaldehyde within 3 min. Under the optimal conditions, the performance of the proposed method was studied in terms of linear dynamic range (10-500 µg/L), correlation coefficient (R(2) ≥ 0.998), precision (RSD% ≤ 5.5) and limit of detection (4 µg/L). Finally, the developed method was successfully applied for extraction and determination of formaldehyde in tap, rain and tomato water samples, and satisfactory results were obtained.
