Polythiophene-coated Fe₃O₄ superparamagnetic nanocomposite: Synthesis and application as a new sorbent for solid-phase extraction

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• 作者：Elham Tahmasebi ; Yadollah Yamini ; ^{yyamini@modares.ac.ir} ; Morteza Moradi ; Ali Esrafili
• 关键词：Polythiophene-coated Fe3O4 magnetic nanoparticles ; Magnetic separation ; Phthalates ; Gas chromatography&ndash ; flame ionization detector ; Solid-phase extraction
• 刊名：Analytica Chimica Acta
• 出版年：2013
• 出版时间：3 April, 2013
• 年：2013
• 卷：770
• 期：Complete
• 页码：68-74
• 全文大小：756 K

文摘

In the present work, a novel type of superparamagnetic nanosorbent, polythiophene-coated Fe₃O₄ nanoparticles (Fe₃O₄@PTh NPs), have been successfully synthesized. The synthesized NPs were characterized by scanning electron microscopy (SEM), Fourier transform-infrared (FT-IR) spectroscopy, and thermal gravimetric analysis (TGA). The synthesized Fe₃O₄@PTh NPs were applied as an efficient sorbent for extraction and preconcentration of several typical plasticizer compounds (di-n-butyl phthalate (DBP), di-(2-ethylhexyl) phthalate (DEHP), and dioctyl adipate (DOA)) from environmental water samples. Separation of Fe₃O₄@PTh NPs from the aqueous solution was simply achieved by applying external magnetic field. Separation and determination of the extracted plasticizers was performed by gas chromatography-flame ionization detection (GC-FID). Several variables affecting the extraction efficiency of the analytes i.e., amount of NPs sorbent, salt concentration, extraction time, and desorption conditions were investigated and optimized. The best working conditions were as follows: amount of sorbent, 100 mg; NaCl concentration, 30 % (w/v); sample volume, 45 mL; extraction time, 10 min; and 100 ¦ÌL of ethyl acetate for desorption of the analytes within 2 min. Under optimized conditions, preconcentration factors for DBP, DEHP, and DOA were obtained as 86, 194, and 213, respectively. The calibration curves were linear (R² > 0.998) in the concentration range of 0.4-100 ¦Ìg L^?1 for both DEHP and DOA and 0.7-100 ¦Ìg L^?1 for DBP. The limits of detection (LODs) were obtained in the range of 0.2-0.4 ¦Ìg L^?1. The intra-day relative standard deviations (RSDs % ) based on four replicates were obtained in the range of 4.0-12.3 % . The proposed procedure was applied to analysis of water samples including river water, bottled mineral water, and boiling water exposed to polyethylene container (after cooling) and recoveries between 85 and 99 % and RSDs lower than 12.8 % were obtained.