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Polyhedral oligomeric silsesquioxanes are 3D nanoscaled materials with large potential in solid phase microextraction (SPME). Here, as a case study, an octaglycidyldimethylsilyl modified polyhedral oligomeric silsesquioxane network is described. It was deposited on a stainless steel wire via a sol-gel method and used as a fiber coating for SPME of aromatic compounds. The uniform pore structure, high surface area, and hydrophobicity of the network make it susceptible toward isolation of non-polar and semi-polar chemical compounds. The performance of the fiber coating was tested with three classes of environmental pollutants, viz. chlorobenzenes (CBs), benzenes (benzene, toluene, ethylbenzene, xylene; known as BTEX), and polycyclic aromatic hydrocarbons. The effects of various types of sol-gel precursors on the fabrication and performance of fiber coatings were investigated. The extraction capability of the fiber coating was compared with the polydimethyl siloxane/divinylbenzene based commercial fiber. Parameters affecting headspace analysis and gas chromatographic quantitation were optimized. The method was applied to the quantification of PAHs, as model analytes, in tea, coffee and some environmental waters. Linear responses typically cover the 1-200 ng·L concentration range, limits of detection are between 0.1 and 0.3 ng·L, intra-day relative standard deviation are <10%, and inter-day RSDs are <12%. The fiber has a long lifespan and can be used >200 times. Graphical abstract Schematic presentation of a headspace solid phase microextraction process which is implemented to the analysis of PAHs in tea and coffee samples. The SEM image of the SPME fiber coating, the 3D nanoscale polyhedral oligomeric silsesquioxane (POSS) network, and the POSS-epoxy molecular structure are shown.

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