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

作者：Abolghasemi Mir Mahdi^*; Hassani Sona; Rafiee Ezzat; Yousefi Vahid

来源：Journal of Chromatography A, 2015, 1381: 48-53.

DOI：10.1016/j.chroma.2014.12.080

• Heteropoly acid
• Polyoxometalate
• gamma-Fe2O3 nanoparticles
• Phenolic compounds
• Solid-phase microextraction
• Gas chromatography-mass spectrometry

In the present study, 12-tungstophosphoric (PW) acid as heteropoly acid, supported on silica-coated gamma-Fe2O3 nanoparticles (NPs), was used as a new fiber coating for solid-phase microextraction (SPME). The gamma-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 0.05 pg mL(-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.

• 出版日期2015-2-13