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Nanoscale-supported heteropoly acid as a new fiber coating for solid-phase microextraction coupled with gas chromatography–mass spectrometry A

Abolghasemi, Mir Mahdi, Hassani, Sona, Rafiee, Ezzat, Yousefi, Vahid
Journal of chromatography 2015 v.1381 pp. 48-53
Fourier transform infrared spectroscopy, coatings, desorption, equipment, ferric oxide, gas chromatography-mass spectrometry, ionic strength, maghemite, mixing, nanocomposites, nanoparticles, pH, phenolic compounds, scanning electron microscopy, solid phase microextraction, stainless steel, statistical analysis, surface area, temperature, thermal stability
In the present study, 12-tungstophosphoric (PW) acid as heteropoly acid, supported on silica-coated γ-Fe2O3 nanoparticles (NPs), was used as a new fiber coating for solid-phase microextraction (SPME). The γ-Fe2O3@SiO2-PW nanocomposite with high surface area was synthesized and characterized by SEM and FT-IR. The prepared nanocomposite was immobilized on a stainless steel wire for fabrication of the SPME fiber. The fiber was evaluated for the extraction of some phenolic compounds (PCs) from water sample in combination with gas chromatography-mass spectrometry (GC-MS). A one-at-a-time optimization strategy was applied for optimizing the important extraction parameters such as extraction temperature, extraction time, ionic strength, stirring rate, pH, and desorption temperature and time. In optimum conditions, the repeatability for one fiber (n=3), expressed as relative standard deviation (R.S.D. %), was between 4.8% and 9.6% for the test compounds. The detection limits for the studied compounds were between 0.004 and 0.05pgmL⁻¹. The developed method offers the advantage of being simple to use, with shorter analysis time, lower cost of equipment, thermal stability of fiber and high relative recovery in comparison to conventional methods of analysis.