Solid phase microextraction has been established as modern analytic method, which provides several benefits such as sensitivity, rapid and solvent free technique for sample preparation in organic analytical chemistry. Nowadays there is a scientific effort dedicated to improve analytical methods based on new and nanostructured materials. Our study follows this trend and contributes to analytical chemistry approach. Explicitly, the investigation of using nanofibrous sorbents for solid phase microextraction.Nanofibres of polyethersulfone (PES), polyetherimide (PEI) and polysulfone (PSU) were successfully prepared by needle electrospinning and fixed on a thin stainless steel wire SPME assmebly. The geometry of sorbents plays a crucial role in the extraction kinetics of the mass transfer in SPME. The intention of using electrospun fibres geometry is to enhance the sorbent sensitivity and capacity.The basic properties of the prepared nanofibers were determined by thermogravimetry (TGA) and scanning electron microscope (SEM). The scanning electron microscopy images of prepared nanofibers showed a diameter range from 700 to 1400 nm for polyethersulfone, 300 to 600 nm for polyetherimide and 800 to 1400 nm for polysulfone. TGA analysis proved the thermal stability of all prepared nanofibers up to 250 °C. The extraction efficiency of new lab-made SPME fibres and selected common commercial SPME fibres (PDMS and PDMS/DVB) was investigated by the headspace SPME (HS-SPME) mode of gas chromatograph coupled with tandem mass spectrometer (GC/MSMS).Hexachlorocyclohexanes isomers (HCH) were selected as model analytes in water matrix. With these pollutants, a set of experiments was conducted to proof the effect of key SPME method conditions extraction time on MSMS response.Keywords: Solid phase microextraction, nanofibres, polyethersulfone, polysulfone, polyetherimide
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